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Article

Laser-Induced Synthesis of Crystalline Silicon Compounds from Aluminum–Silica–Carbon Powder

by
Andrey Ivanovich Gorodov
,
Vyacheslav Ivanovich Pavlenko
,
Daria Alexandrovna Sinebok
,
Natalia Igorevna Cherkashina
,
Roman Nikolaevich Yastrebinsky
*,
Anna Viktorovna Yastrebinskaya
and
Nadezhda Ivanovna Bondarenko
Department of Theoretical and Applied Chemistry, Belgorod State Technological University Named After V.G. Shukhov, 308012 Belgorod, Russia
*
Author to whom correspondence should be addressed.
J. Compos. Sci. 2025, 9(12), 643; https://doi.org/10.3390/jcs9120643
Submission received: 24 October 2025 / Revised: 21 November 2025 / Accepted: 25 November 2025 / Published: 26 November 2025
(This article belongs to the Section Composites Manufacturing and Processing)
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Abstract

The paper investigates the feasibility of laser-induced synthesis of crystalline silicon compounds from a powder system consisting of metallic aluminum, amorphous silica, and carbon atoms. Using pulsed laser radiation (wavelength 1064 nm), it is experimentally demonstrated that varying the processing parameters—pulse energy, repetition rate, scanning speed, and pulse duration—allows for targeted control of the phase composition of the products. Modes for the selective formation of crystalline silicon, mullite, and intermediate acid-soluble aluminosilicates are established. Using a simplified thermal model, a correlation is demonstrated between the achieved temperature in the irradiation zone and the formation of specific phases, with not only the peak temperature at the laser point but also the exposure time playing a key role. It is shown that crystalline acid-soluble silicate phases preceded the formation of mullite. The results of low-temperature laser synthesis of crystalline silicon-containing materials hold great promise for various applications.

1. Introduction

Optical energy, controlled by modern laser sources, is a powerful tool enabling innovative approaches to high-precision material processing. These technologies are widely used in high-tech industries such as micro- and nano-engineering, electronics, optoelectronics, as well as in biomedical engineering and the development of new materials [1,2].
Among the various laser processing methods, the use of ultrashort pulses—femtosecond and picosecond—occupies a special place, opening up new horizons in nanostructuring and mechanical micromachining. One such technology is femtosecond laser ablation [3], capable of processing materials with nanometer precision without thermal impact on adjacent areas. This method is particularly effective when working with transparent and difficult-to-machine materials [4]. Laser processing of materials typically involves laser ablation—a process in which material is removed by localized vaporization under the influence of laser energy exceeding a certain threshold flux density. However, at energies below the ablation threshold, other photoinduced effects are possible, including structural and chemical modifications such as melting [5], oxidation [6], and modification of defect structures, which also manifest themselves when the appropriate threshold conditions are reached.
One of the most important areas of laser processing is the induction of phase transitions, in particular, the crystallization of amorphous materials. Laser crystallization, or laser annealing, is currently widely used in semiconductor manufacturing, including the creation of thin-film systems based on polycrystalline silicon (poly-Si), used in active matrices of flat-panel displays, as well as in photovoltaic devices. Polycrystalline silicon plays a key role in solar energy technologies: it is used as the active and passivation layer in solar cells based on monocrystalline silicon (c-Si). Furthermore, polysilicon is widely used in vertically integrated memory devices.
Among the many approaches to crystallizing amorphous silicon—such as thermal annealing, solid-state crystallization, metal-induced crystallization, and sequential lateral solidification—laser annealing, particularly using excimer and femtosecond lasers, has gained the greatest research and technological significance [7,8,9,10,11], this method also offers several advantages over existing approaches, namely: localized energy input and reduced overall thermal impact on the system; the ability to selectively control the phase composition by adjusting the pulse parameters; and the formation of crystalline silicon at lower temperatures without the need to heat the entire volume of material. These features make laser synthesis a promising low-energy method for the production of silicon-containing materials. Laser annealing involves short-term and localized heating of the amorphous silicon surface to the phase transition temperature, followed by rapid cooling and formation of the crystalline phase [12,13]. Due to the extremely short exposure times achieved using femtosecond pulses, this process avoids substrate overheating, which is critical when working with temperature-sensitive materials.
Femtosecond laser annealing (FLA) exhibits a number of advantages over other methods: selective heating of a specific layer in a multilayer structure, the ability to process complex multilayer structures, and the ability to simultaneously crystallize and modify the surface [4,14,15,16,17,18,19,20,21]. Ultrafast laser-induced crystallization, or FLA, of amorphous silicon films has been extensively studied over the past decade. Using time-resolved pump-probe spectroscopy, Choi [22] et al. showed that crystallization begins with the formation of defects and growth nuclei induced by ultrafast nonthermal stimulation, followed by melting and explosive crystallization on nanosecond time scales. This mechanism has been confirmed by subsequent studies and modeling, including molecular dynamics [23,24].
Femtosecond annealing also modifies the optical and electrical characteristics of the processed films: the refractive index, absorption coefficient, and transition type (direct or indirect) are altered, conductivity increases, and impurities are activated through substitution in the crystal lattice. It has also been noted that spatially selective crystallization leads to the formation of nanostructured silicon with improved absorption in the near-IR range [17,18] and increased electrical conductivity [19] when doped with boron, making such structures particularly promising for photovoltaic applications. In addition to the changes described in film systems, recent attention has also been focused on laser-induced transformations in powder and composite systems, where local pulsed radiation initiates solid-state or thermochemical reactions between components. It has been shown that laser processing of oxide and silicate powders leads to melting and sintering, allowing the production of crystalline products [25,26,27].
Despite numerous studies devoted to femtosecond and picosecond laser crystallization, the fundamental principles of laser-induced phase transformation—localized heating, rapid cooling, and nonequilibrium solidification—remain relevant over a wide range of pulse durations. In this paper, these principles are applied to nanosecond laser irradiation of a powder system.
Another common method for producing polycrystalline silicon is based on the chemical reaction of silicon oxide reduction with aluminum, carried out at high temperatures (over 1100 °C) [28]. However, the development of modern industry requires lower-temperature conditions for producing crystalline silicon. In our previous studies [29,30], we demonstrated the possibility of producing polycrystalline silicon by low-temperature annealing (550–700 °C) of powder systems consisting of finely dispersed aluminum particles and amorphous silica–carbon material. Moreover, the formation of crystalline silicon from a powder obtained from a mixture of organosilicon compounds and aluminum at a relatively low temperature is possible only in the presence of carbon atoms. We have shown that the reaction begins in the region of solid-phase interaction of particles and largely depends on the processes occurring at the phase boundary. Therefore, the use of focused laser radiation is one of the promising approaches for the thermochemical or photochemical initiation of this chemical reaction.
In contrast to studies devoted to laser crystallization of thin films, the present work investigates the process of laser-induced solid-state synthesis in an aluminum–silica–carbon powder system, in which localized pulsed irradiation initiates coupled thermochemical reactions. This approach makes it possible to form crystalline silicon at significantly lower temperatures than those required in conventional furnace synthesis and enables the production of targeted phase compositions in powder systems using compact nanosecond lasers.
The aim of this work is to establish the possibility of obtaining crystalline silicon compounds from Aluminum–Silica–Carbon powder under the action of local high-intensity laser radiation and to study the influence of laser annealing parameters (pulse energy, modulation frequency, scanning speed, number of passes) on the phase composition of the products.

2. Materials and Methods

2.1. Materials

Aluminum–Silica–Carbon powder (ASC-powder) was obtained by pyrolysis of a dispersion consisting of aluminum particles and organosilicon liquid at a temperature of 280 °C, according to a previously developed technique [29,30]. Polyethylhydrosiloxane (PEHS) (LLC Point, Moscow, Russia) was used as the initial organosilicon material. Aluminum powder of the PAP-2 brand (LLC Novosverdlovsk Metallurgical Company, Ekaterinburg, Russia) consisting of irregularly shaped particles with a diameter of 20–30 μm and a thickness of 0.1–0.8 μm, coated with a thin layer of stearin, was also used in the work. The aluminum content in the obtained ASC-powder is ~10 wt%.

2.2. Research Methods

After homogenization in a ceramic mortar, the aluminum–silica–carbon powder was placed in a thin layer between two glasses to prevent particle removal by heat and air currents. Laser processing was performed using a Minimarker 2-20 A4 PA system (Laser Center, St. Petersburg, Russia) equipped with an ytterbium-doped pulsed fiber laser with a primary wavelength of 1064 nm and a maximum output power of 20 W. The laser beam was focused onto a spot 8–10 μm in diameter on the powder surface. Powder processing was performed on both sides at a room temperature of 25 °C in an atmospheric environment.
Thermophysical constants of the ASC powder used in thermal calculations were determined using a KIT-Nanocomposite computerized thermal conductivity meter (DB Teplofon, Moscow, Russia). The instrument’s operating principle is based on preheating the sample, followed by monotonic cooling and recording of the cooling process. During the cooling phase, the thermal conductivity and heat capacity of the sample are scanned at a set temperature increment of 10 °C.
X-ray diffraction was used to identify the crystalline phases present in the obtained powders. The studies were conducted using an ARL X’TRA’A instrument (LLC Thermotechno, Geneve, Switzerland) in asymmetric coplanar mode with a grazing incidence angle of α = 3° (θ-scan). The X-ray spectra were compared with data from the Powder Diffraction File (PDF) database of the ICDD (International Centre for Diffraction Data, Newtown Square, PA, USA) and COD (Crystallography Open Database).
The products obtained after laser treatment were studied by scanning electron microscopy (SEM) with the removal of energy-dispersive X-ray spectra (EDS). The studies were performed using a high-resolution scanning electron microscope TESCAN MIRA 3LMU with an integrated X-MAX 50 energy dispersion spectrometer from Oxford Instruments (TESCAN ORSAY HOLDING, Brno, Czech Republic).

3. Results and Discussion

To study the influence of laser radiation parameters on the composition of the crystalline phases of the resulting products, samples were processed at different values of single-pulse energy (Ep, μJ), number of laser pulses (f, kHz), beam speed (V, mm/s), and pulse width (Pw, ns). X-ray diffraction patterns of the original ASC powder and samples obtained as a result of a single pass (n = 1) of the laser beam over their surface are shown in Figure 1.
The X-ray spectra of the initial ASC powder (Figure 1a) are characterized by the presence of crystalline phases of aluminum (PDF card No. 85-1327) and two amorphous halos: carbon-containing phase C (2θ = 6.5–12°) and silica SiO2 (2θ = 18–30°) [29,30,31]. Analysis of the X-ray diffraction patterns of ASC-powder after laser processing (Figure 1b–j) showed that, depending on the laser scanning parameters, various chemical processes are initiated with the formation of different crystalline products: silicon Si (PDF card No. 75-589), Al2O3 (PDF card No. 17-1862), mullite 3Al2O3∙SiO2 (PDF card No. 79-1450) and other aluminum silicates AlxSiyOz (with interplanar spacing d = 10.901–10.522 Å). However, in some diffraction patterns (Figure 1b–g), an amorphous silica halo is preserved in the region of angles 2θ = 15–25°, while changes in its shape and displacement are observed, depending on the laser mode used. The X-ray spectra of almost all samples also contain signals corresponding to the crystalline phase of aluminum, indicating that chemical reactions are incomplete. One of the possible reasons for the incomplete reaction between amorphous silica and aluminum during laser treatment is the low penetration of the laser beam deep into the material and, consequently, the small heat exposure zone. Another important reason is the short duration of the process.
To elucidate the thermal role of laser irradiation on the resulting crystalline products, the surface heating temperature at the point of contact with the laser beam was estimated using the parameters of the laser radiation flux absorbed by the substance (as a heat source), as well as the thermophysical constants of ASC powder, SiO2, and Al. Solving the heat conduction equation is generally very complex [27,32]. We used a simplified model based on heat conduction equations without taking into account hydrodynamic, gasdynamic, and plasma processes, phase transitions, the temperature dependence of heat capacity and thermal conductivity, etc. The temperature profile during heating with a laser heat source was determined solely by heat transfer processes due to thermal conductivity, taking into account the laser heat flux (distribution was Gaussian) and heat loss due to radiation and convection. The model used does not claim to provide a precise quantitative description of the temperatures achieved but rather provides an approximate prediction of thermal heating in the system.
Figure 2 shows the calculated temperature at the laser scanning point of the ASC powder surface under various processing parameters. It is evident that the temperature on the particle surface quickly reaches a maximum and then slowly decreases immediately after the pulse. The obtained heating mechanisms are consistent with the X-ray phase analysis data. For example, in samples processed with a laser beam of high pulse energy (Ep = 20 μJ) or at a low travel speed (V = 10 mm/s), mullite-type aluminosilicates are formed (Figure 1b–d). Moreover, the calculated temperature during a beam path of 1.5 μm (which is smaller than the laser spot of d = 8 μm) exceeds 1200 °C (Figure 2a–c). At the same time, the temperature of synthetic formation of mullite is T > 1000 °C [33].
The highest mullite content was obtained with the laser processing mode Ep = 20 μJ, f = 1000 kHz, V = 10 mm/s, Pw = 8 ns (Figure 1b), at which the highest temperature was achieved (Figure 2a). With a decrease in the achieved temperature (Figure 2b,c), due to a decrease in the energy of one pulse and the beam travel speed, the mullite content decreases, as evidenced by a decrease in the relative signal intensity in the X-ray diffraction patterns (Figure 1c,d).
Temperatures T > 1200 °C are also achieved when the laser beam travels a path of 1.5 μm with the processing mode Ep = 4 μJ, f = 500 kHz, V = 120 mm/s, Pw = 4 ns (Figure 2f), but the formation of the crystalline phase of mullite does not occur (Figure 1g). Apparently, this is due to the fact that the temperature regime is not maintained for the required time, since the beam travels a path of 1.5 μm in 12.5 μs, which is 12 times less than at a travel speed of 10 mm/s. However, in this laser scanning mode, a new peak with d = 10.855 Å was recorded in the X-ray diffraction pattern, which could not be accurately identified due to the overlap of diffraction signals with reflections from other crystalline and amorphous components of the system. We assume the formation of silicates of the ferrierite type, consisting entirely of silica SiO2-FER (PDF card No. 82-1395) [34,35], or aluminosilicates of a layered structure, where the distance corresponds to the layer repetition period in the crystal lattice of Al4Si8O22 (COD card No. 1530329) or Al15.68(Si41Al6.9)O96 (COD card No. 8103693). The formation of similar substances (Figure 1e,f,j) also occurs under other laser processing modes, where the temperature achieved at the scanning point is lower (Figure 2d,e,i). A slight fluctuation in the interplanar spacing values is apparently due to the difference in the crystal structure of the substances formed at different temperatures.
At low pulse energy (Ep = 0.4 μJ) but slow scanning speed (V = 75 mm/s), a more gradual increase in the surface temperature of the ASC powders occurs as the laser moves (Figure 2d). In this case, the intensity of the diffraction maximum d = 10.855 Å, and hence the silicate content, is higher (Figure 1e), compared to laser processing modes with higher pulse energy but higher speed (Figure 1f–h,j). With increasing laser speed, at the same pulse energy levels, the intensity of the X-ray peaks decreases to traces (Figure 1h vs. Figure 1g) or the signals of these silicates disappear completely (Figure 1i vs. Figure 1f). Obviously, this is due to a change in the average temperature of the material in the scanning area.
At the optimal conditions Ep = 2.8 μJ, f = 500 kHz, V = 330 mm/s, Pw = 4 ns, only crystalline silicon is formed (Figure 1i). With increasing laser temperature (when the material temperature after 1 pulse is >250 °C), both due to an increase in energy (Figure 2g vs. Figure 2h) and the duration of one pulse (Figure 2i vs. Figure 2h), the formation of silicates with d = 10.855 Å occurs (Figure 1h,j).
With an increasing number of laser passes, in the mode Ep = 0.4 μJ, f = 500 kHz, V = 75 mm/s, Pw = 4 ns, the intensity of the X-ray peak in the region of the angle 2θ ≈ 9.5° decreases, but traces of mullite phases appear (Figure 3a vs. Figure 1e). However, in modes with a higher laser travel speed, despite the higher pulse energy, clear signals characteristic of the mullite phase are absent in the X-ray diffraction pattern of the products (Figure 3b–d). Perhaps this is due to insufficient time or temperature conditions of laser processing. Also, with an increase in the number of laser passes, with unchanged processing parameters, the intensity of X-ray signals of crystalline phases of silicon decreases (Figure 3a–d vs. Figure 1e,f,h,i, respectively). At the same time, if we first treat the sample with a single laser pass in the mode Ep = 2.8 μJ, f = 500 kHz, V = 330 mm/s, Pw = 4 ns (Figure 1i), and then repeat with a lower pulse energy, the formation of silicates with d = 10.855 Å is intensified (Figure 4). This and the data presented above indicate that the formed crystalline phase of these silicates is intermediate before the formation of mullite.
Silicates obtained under different conditions, exhibiting an X-ray peak near 2θ ≈ 9.5°, were treated with concentrated hydrochloric acid (HCl) at 80 °C for 20 min under continuous stirring, using a liquid-to-solid ratio of 5:1 and then washed with distilled water. The X-ray diffraction patterns were similar. It is evident (Figure 5) that the silicates and aluminum were completely dissolved, while crystalline silicon and amorphous SiO2 remained in the system. Thus, silicates with d = 10.855 Å are acid-soluble.
Micrographs of products obtained as a result of ASC-powders laser treatment revealed aggregates of nanoscale (~50nm) spherical particles (Figure 6a), which apparently belong to crystalline silicon. There are also cellular (layered) formations (Figure 6b) of aluminosilicates. Filamentous growths of aluminosilicates (mullite) surrounded by spherical aggregates adjoin some sections of the cells (Figure 6c). This confirms the previously described results that the formation of mullite occurs after the formation of layered silicates.

4. Conclusions

Pulsed local laser irradiation is an effective method for initiating chemical transformations in the Al–SiO2–C system, leading to the formation of various crystalline phases, including silicon (Si), mullite (3Al2O3 2SiO2), and acid-soluble layered aluminosilicates. The phase composition of the reaction products depends on the laser processing parameters: pulse energy, pulse repetition rate, scanning speed, and pulse duration. High temperatures (>1200 °C), achieved at high pulse energies and low laser travel speeds, promote mullite formation. Under non-optimal laser processing parameters, depending on the operating conditions, several reaction products are formed simultaneously. Under optimal conditions, for example (Ep = 2.8 μJ, f = 500 kHz, V = 330 mm/s, Pw = 4 ns), it is possible to selectively obtain crystalline silicon. An acid-soluble layered aluminum silicate phase was discovered. It forms when the powder surface temperature at the point of contact with the laser beam is higher than the laser point temperature during crystalline silicon formation. Mullite forms during subsequent laser-thermal treatment.
Modeling of temperature fields confirmed the correlation between the temperature achieved in the irradiation zone and the formation of specific crystalline phases. However, not only the peak temperature but also the laser-thermal exposure time are critical for phase formation. Multi-pass laser treatment changes the phase composition of the product, intensifying the formation of aluminosilicates and reducing the crystalline silicon content, indicating the complex multi-stage nature of the processes.
Laser-induced synthesis of crystalline silicon compounds from aluminum–silica–carbon powder has shown great promise for the controlled low-temperature synthesis of target crystalline silicon phases and aluminosilicates from aluminum–silica–carbon powder. This work has important practical significance for the production of materials containing crystalline silicon systems, in particular in the ceramic industry, the production of refractory materials, lithium–silicon batteries, biological products and other areas of industry.

Author Contributions

Conceptualization, V.I.P.; Formal analysis, N.I.C. and A.V.Y.; Investigation, A.I.G., D.A.S., N.I.C., A.V.Y. and N.I.B.; Methodology, R.N.Y. and N.I.B.; Resources, R.N.Y.; Supervision, V.I.P.; Writing—original draft, D.A.S.; Writing—review & editing, A.I.G. All authors have read and agreed to the published version of the manuscript.

Funding

This work was realized using the equipment of the High Technology Center at BSTU named after V.G. Shukhov, the framework of the State Assignment of the Ministry of Education and Science of the Russian Federation, project No. FZWN-2023-0004.

Data Availability Statement

The data presented in this study are available from the corresponding author upon reasonable request.

Conflicts of Interest

The authors declare no conflicts of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, or in the decision to publish the results.

References

  1. Belaforte, D.A. The global market for industrial laser processing. Photonics Views 2020, 17, 35–37. [Google Scholar] [CrossRef]
  2. Bonse, J.; Lasagni, A.F. Laser micro- and nano-material processing—Part 1. Adv. Opt. Technol. 2020, 9, 7–9. [Google Scholar] [CrossRef]
  3. Liu, X.; Du, D.; Mourou, G. Laser ablation and micromachining with ultrashort laser pulses. IEEE J. Quantum Electron. 1997, 33, 1706. [Google Scholar] [CrossRef]
  4. Gattass, R.R.; Mazur, E. Femtosecond laser micromachining in transparent materials. Nat. Photonics 2008, 2, 219. [Google Scholar] [CrossRef]
  5. Bäuerle, D. Laser Processing and Chemistry, 4th ed.; Springer: Berlin/Heidelberg, Germany, 2011. [Google Scholar]
  6. Bonse, J.; Sturm, H.; Schmidt, D.; Kautek, W. Chemical, morphological and accumulation phenomena in ultrashort-pulse laser ablation of TiN in air. Appl. Phys. A 2000, 71, 657–665. [Google Scholar] [CrossRef]
  7. Im, J.S.; Kim, H.J.; Thompson, M.O. Phase transformation mechanisms involved in excimer laser crystallization of amorphous silicon films. Appl. Phys. Lett. 1993, 63, 1969–1971. [Google Scholar] [CrossRef]
  8. Miyasaka, M.; Stoemenos, J. Excimer laser annealing of amorphous and solid-phase-crystallized silicon films. J. Appl. Phys. 1999, 86, 5556–5565. [Google Scholar] [CrossRef]
  9. Smith, P.M.; Carey, P.G.; Sigmon, T.W. Excimer laser crystallization and doping of silicon films on plastic substrates. Appl. Phys. Lett. 1997, 70, 342–344. [Google Scholar] [CrossRef]
  10. Song, D.; Inns, D.; Straub, A.; Terry, M.L.; Campbell, P.; Aberle, A.G. Solid phase crystallized polycrystalline thin-films on glass from evaporated silicon for photovoltaic applications. Thin Solid Film. 2006, 513, 356–363. [Google Scholar] [CrossRef]
  11. Sameshima, T.; Usui, S.; Sekiya, M. XeCl Excimer laser annealing used in the fabrication of poly-Si TFT’s. IEEE Electron Device Lett. 1986, 7, 276–278. [Google Scholar] [CrossRef]
  12. Marqués, L.A.; Pelaz, L.; Aboy, M.A.; Barbolla, J. The laser annealing induced phase transition in silicon: A molecular dynamics study. Nucl. Instrum. Methods Phys. Res. Sect. B 2004, 216, 57–61. [Google Scholar] [CrossRef]
  13. Goto, T.; Saito, K.; Imaizumi, F.; Hatanaka, M.; Takimoto, M.; Mizumura, M.; Gotoh, J.; Ikenoue, H.; Sugawa, S. LTPS Thin-Film Transistors Fabricated Using New Selective Laser Annealing System. IEEE Trans. Electron Devices 2018, 65, 3250–3256. [Google Scholar] [CrossRef]
  14. Phillips, K.C.; Gandhi, H.H.; Mazur, E.; Sundaram, S.K. Ultrafast laser processing of materials: A review. Adv. Opt. Photonics 2015, 7, 684–712. [Google Scholar] [CrossRef]
  15. Arduino, D.; Stassi, S.; Spano, C.; Scaltrito, L.; Ferrero, S.; Bertana, V. Silicon and Silicon Carbide Recrystallization by Laser Annealing: A Review. Materials 2023, 16, 7674. [Google Scholar] [CrossRef] [PubMed]
  16. Theodorakos, I.; Zergioti, I.; Vamvakas, V.; Tsoukalas, D.; Raptis, Y.S. Picosecond and nanosecond laser annealing and simulation of amorphous silicon thin films for solar cell applications. J. Appl. Phys. 2014, 115, 043108. [Google Scholar] [CrossRef]
  17. Nayak, B.K.; Gupta, M.C. Femtosecond-laser-induced-crystallization and simultaneous formation of light trapping microstructures in thin a-Si:H films. Appl. Phys. A 2007, 89, 663. [Google Scholar] [CrossRef]
  18. Wang, X.C.; Zheng, H.Y.; Tan, C.W.; Wang, F.; Yu, H.Y.; Pey, K.L. Femtosecond laser induced surface nanostructuring and simultaneous crystallization of amorphous thin silicon film. Opt. Express 2010, 18, 19379. [Google Scholar] [CrossRef]
  19. Pavlikov, A.V.; Forsh, P.A.; Svyakhovskiy, S.E.; Matsukatova, A.N.; Forsh, E.A.; Kazanskii, A.G.; Kashkarov, P.K. Giant enhancement of free charge carrier concentration in boron-doped amorphous hydrogenated silicon under femtosecond laser crystallization. Appl. Phys. Lett. 2018, 113, 203103. [Google Scholar] [CrossRef]
  20. Li, D.; Ilyas, N.; Song, Y.; Zhong, H.; Li, W.; Jiang, Y. Inhomogeneous crystallization of a-Si thin films irradiated by femtosecond laser. J. Raman Spectrosc. 2019, 50, 793. [Google Scholar] [CrossRef]
  21. Torregrosa, F.; Canino, M.; Li, F.; Tamarri, F.; Roux, B.; Morata, S.; La Via, F.; Zielinski, M.; Nipoti, R. Ion implantation and activation of aluminum in bulk 3C-SiC and 3C-SiC on Si. MRS Adv. 2022, 7, 1347–1352. [Google Scholar] [CrossRef]
  22. Choi, T.Y.; Hwang, D.J.; Grigoropoulos, C.P. Ultrafast laser-induced crystallization of amorphous silicon films. Opt. Eng. 2003, 42, 3383. [Google Scholar] [CrossRef]
  23. Volodin, V.A.; Efremov, M.D.; Kachurin, G.A.; Cherkov, A.G.; Deutschmann, M.; Baersch, N. Phase transitions in a-Si:H films on a glass irradiated by high-power femtosecond pulses: Manifestation of nonlinear and nonthermal effects. JETP Lett. 2007, 86, 119. [Google Scholar] [CrossRef]
  24. Izawa, Y.; Tokita, S.; Fujita, M.; Norimatsu, T.; Izawa, Y. Ultra fast melting process in femtosecond laser crystallization of thin a-Si layer. Appl. Surf. Sci. 2009, 255, 9764. [Google Scholar] [CrossRef]
  25. Maeng, S.H.; Lee, H.; Park, M.S.; Park, S.; Jeong, J.; Kim, S. Ultrafast carbothermal reduction of silica to silicon using a CO2 laser beam. Sci. Rep. 2020, 10, 21730. [Google Scholar] [CrossRef]
  26. Wu, D.; Zhao, D.; Niu, F.; Huang, Y.; Zhu, J.; Ma, G. In situ synthesis of melt-grown mullite ceramics using directed laser deposition. J. Mater. Sci. 2020, 55, 12761–12775. [Google Scholar] [CrossRef]
  27. Smirnov, A.A.; Pikulin, A.; Sapogova, N.; Bityurin, N. Femtosecond Laser Irradiation of Plasmonic Nanoparticles in Polymer Matrix: Implications for Photothermal and Photochemical Material Alteration. Micromachines 2014, 5, 1202–1218. [Google Scholar] [CrossRef]
  28. Lavrov, N.N.; Lavrov, B.A.; Serzhanov, G.M. Preparation of polycrystalline silicon by the aluminothermic method. News St. Petersburg State Technol. Inst. Tech. Univ. 2015, 31, 30–32. (In Russian) [Google Scholar]
  29. Pavlenko, V.I.; Gorodov, A.I.; Cherkashina, N.I.; Ryzhikh, D.A.; Ruchii, A.Y. Influence of Temperature of Silicon Dioxide Powder Annealing on the Aluminum-Induced Crystallization of Polycrystalline Silicon. Russ. J. Appl. Chem. 2023, 96, 838–846. [Google Scholar] [CrossRef]
  30. Cherkashina, N.I.; Pavlenko, V.I.; Gorodov, A.I.; Ryzhikh, D.A. Preparation of Polycrystalline Silicon by Metal-Induced Crystallization of Silicon–Carbon Powder. Ceramics 2024, 7, 989–1001. [Google Scholar] [CrossRef]
  31. Pavlenko, V.I.; Cherkashina, N.I.; Edamenko, O.D.; Yastrebinsky, R.N.; Noskov, A.V.; Prokhorenkov, D.S.; Gorodov, A.I.; Piskareva, A.O. Synthesis and Characterization of Silicon–Carbon Powder and Its Resistance to Electron Irradiation. J. Compos. Sci. 2023, 7, 340. [Google Scholar] [CrossRef]
  32. Vora, H.D.; Santhanakrishnan, S.; Harimkar, S.P.; Boetcher, S.K.S.; Dahotre, N.B. One-dimensional multipulse laser machining of structural alumina: Evolution of surface topography. Int. J. Adv. Manuf. Technol. 2013, 68, 69–83. [Google Scholar] [CrossRef]
  33. Abdullayev, A.; Zemke, F.; Gurlo, A.; Bekheet, M.F. Low-temperature fluoride-assisted synthesis of mullite whiskers. RSC Adv. 2020, 10, 31180–31186. [Google Scholar] [CrossRef]
  34. Arletti, R.; Fois, E.; Gigli, L.; Vezzalini, G.; Quartieri, S.; Tabacchi, G. Irreversible Conversion of a Water–Ethanol Solution into an Organized Two-Dimensional Network of Alternating Supramolecular Units in a Hydrophobic Zeolite under Pressure. Angew. Chem. Int. Ed. 2017, 56, 2105–2109. [Google Scholar] [CrossRef]
  35. Rakoczy, R.A.; Traa, Y.; Kortunov, P.; Vasenkov, S.; Kärger, J.; Weitkamp, J. Synthesis of large crystals of all-silica zeolite ferrierite. Microporous Mesoporous Mater. 2007, 104, 179–184. [Google Scholar] [CrossRef]
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Figure 1. X-ray diffraction patterns of ASC-powder samples before and after laser treatment under different conditions: (a) No Laser; (b) Ep = 20 μJ, f = 1000 kHz, V = 10 mm/s, Pw = 8 ns; (c) Ep = 0.4, f = 500, V = 10, Pw = 4; (d) Ep = 0.8, f = 250, V = 10, Pw = 4; (e) Ep = 0.4, f = 500, V = 75, Pw = 4; (f) Ep = 2.8, f = 500, V = 315, Pw = 4; (g) Ep = 4, f = 500, V = 120, Pw = 4; (h) Ep = 4, f = 500, V = 350, Pw = 4; (i) Ep = 2.8, f = 500, V = 330, Pw = 4; (j) Ep = 2.8, f = 500, V = 330, Pw = 50.
Figure 1. X-ray diffraction patterns of ASC-powder samples before and after laser treatment under different conditions: (a) No Laser; (b) Ep = 20 μJ, f = 1000 kHz, V = 10 mm/s, Pw = 8 ns; (c) Ep = 0.4, f = 500, V = 10, Pw = 4; (d) Ep = 0.8, f = 250, V = 10, Pw = 4; (e) Ep = 0.4, f = 500, V = 75, Pw = 4; (f) Ep = 2.8, f = 500, V = 315, Pw = 4; (g) Ep = 4, f = 500, V = 120, Pw = 4; (h) Ep = 4, f = 500, V = 350, Pw = 4; (i) Ep = 2.8, f = 500, V = 330, Pw = 4; (j) Ep = 2.8, f = 500, V = 330, Pw = 50.
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Figure 2. Dependence of temperature at the point of laser irradiation on the laser advancement for different processing parameters: (a) Ep = 20 μJ, f = 1000 kHz, V = 10 mm/s, Pw = 8 ns; (b) Ep = 0.4, f = 500, V = 10, Pw = 4; (c) Ep = 0.8, f = 250, V = 10, Pw = 4; (d) Ep = 0.4, f = 500, V = 75, Pw = 4; (e) Ep = 2.8, f = 500, V = 315, Pw = 4; (f) Ep = 4, f = 500, V = 120, Pw = 4; (g) Ep = 4, f = 500, V = 350, Pw = 4; (h) Ep = 2.8, f = 500, V = 330, Pw = 4; (i) Ep = 2.8, f = 500, V = 330, Pw = 50.
Figure 2. Dependence of temperature at the point of laser irradiation on the laser advancement for different processing parameters: (a) Ep = 20 μJ, f = 1000 kHz, V = 10 mm/s, Pw = 8 ns; (b) Ep = 0.4, f = 500, V = 10, Pw = 4; (c) Ep = 0.8, f = 250, V = 10, Pw = 4; (d) Ep = 0.4, f = 500, V = 75, Pw = 4; (e) Ep = 2.8, f = 500, V = 315, Pw = 4; (f) Ep = 4, f = 500, V = 120, Pw = 4; (g) Ep = 4, f = 500, V = 350, Pw = 4; (h) Ep = 2.8, f = 500, V = 330, Pw = 4; (i) Ep = 2.8, f = 500, V = 330, Pw = 50.
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Figure 3. X-ray diffraction patterns of ASC-powder samples after treatment with several laser passes under different conditions: (a) Ep = 0.4 μJ, f = 500 kHz, V = 75 mm/s, Pw = 4 ns, n = 5; (b) Ep = 2.8, f = 500, V = 315, Pw = 4, n = 5; (c) Ep = 4, f = 500, V = 350, Pw = 4, n = 2; (d) Ep = 2.8, f = 500, V = 330, Pw = 4, n = 2.
Figure 3. X-ray diffraction patterns of ASC-powder samples after treatment with several laser passes under different conditions: (a) Ep = 0.4 μJ, f = 500 kHz, V = 75 mm/s, Pw = 4 ns, n = 5; (b) Ep = 2.8, f = 500, V = 315, Pw = 4, n = 5; (c) Ep = 4, f = 500, V = 350, Pw = 4, n = 2; (d) Ep = 2.8, f = 500, V = 330, Pw = 4, n = 2.
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Figure 4. X-ray diffraction patterns of ASC-powder samples after initial laser irradiation at Ep = 2.8 μJ, f = 500 kHz, V = 330 mm/s, Pw = 4 ns and subsequent processing at: (a) Ep = 1.4, f = 500, V = 330, Pw = 4, n = 1; (b) Ep = 0.4, f = 500, V = 350, Pw = 4, n = 1.
Figure 4. X-ray diffraction patterns of ASC-powder samples after initial laser irradiation at Ep = 2.8 μJ, f = 500 kHz, V = 330 mm/s, Pw = 4 ns and subsequent processing at: (a) Ep = 1.4, f = 500, V = 330, Pw = 4, n = 1; (b) Ep = 0.4, f = 500, V = 350, Pw = 4, n = 1.
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Figure 5. X-ray diffraction pattern of the ASC-powder sample after initial laser irradiation at Ep = 0.4 μJ, f = 500 kHz, V = 75 mm/s, Pw = 4 ns, n = 1 and subsequent treatment with hydrochloric acid.
Figure 5. X-ray diffraction pattern of the ASC-powder sample after initial laser irradiation at Ep = 0.4 μJ, f = 500 kHz, V = 75 mm/s, Pw = 4 ns, n = 1 and subsequent treatment with hydrochloric acid.
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Figure 6. SEM images of ASC-powder after laser exposure: (a) crystalline silicon phase; (b) layered silicates; (c) mullite phase.
Figure 6. SEM images of ASC-powder after laser exposure: (a) crystalline silicon phase; (b) layered silicates; (c) mullite phase.
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Gorodov, A.I.; Pavlenko, V.I.; Sinebok, D.A.; Cherkashina, N.I.; Yastrebinsky, R.N.; Yastrebinskaya, A.V.; Bondarenko, N.I. Laser-Induced Synthesis of Crystalline Silicon Compounds from Aluminum–Silica–Carbon Powder. J. Compos. Sci. 2025, 9, 643. https://doi.org/10.3390/jcs9120643

AMA Style

Gorodov AI, Pavlenko VI, Sinebok DA, Cherkashina NI, Yastrebinsky RN, Yastrebinskaya AV, Bondarenko NI. Laser-Induced Synthesis of Crystalline Silicon Compounds from Aluminum–Silica–Carbon Powder. Journal of Composites Science. 2025; 9(12):643. https://doi.org/10.3390/jcs9120643

Chicago/Turabian Style

Gorodov, Andrey Ivanovich, Vyacheslav Ivanovich Pavlenko, Daria Alexandrovna Sinebok, Natalia Igorevna Cherkashina, Roman Nikolaevich Yastrebinsky, Anna Viktorovna Yastrebinskaya, and Nadezhda Ivanovna Bondarenko. 2025. "Laser-Induced Synthesis of Crystalline Silicon Compounds from Aluminum–Silica–Carbon Powder" Journal of Composites Science 9, no. 12: 643. https://doi.org/10.3390/jcs9120643

APA Style

Gorodov, A. I., Pavlenko, V. I., Sinebok, D. A., Cherkashina, N. I., Yastrebinsky, R. N., Yastrebinskaya, A. V., & Bondarenko, N. I. (2025). Laser-Induced Synthesis of Crystalline Silicon Compounds from Aluminum–Silica–Carbon Powder. Journal of Composites Science, 9(12), 643. https://doi.org/10.3390/jcs9120643

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