Home – Home – Jornals – Chemistry for Sustainable Development 2025 number 6

2025 was an anniversary year for the Federal Research Center of Coal and Coal Chemistry of the Siberian Branch of the Russian Academy of Sciences (FRC CCC SB RAS, Kemerovo), and in 2024, the Institute of Coal Chemistry and Material Science (ICCMS), which is now part of FRC CCC SB RAS, celebrated its 50th anniversary. The chronology of the ICCMS formation is presented below. From October 7 to 9, 2025, the city of Kemerovo hosted the 14th International Russian-Kazakhstani Symposium “Carbon Chemistry and Ecology of Kuzbass”, dedicated to the 10th anniversary of FRC CCC SB RAS. This issue of the journal “Chemistry for Sustainable Development” presents materials on the best presentations of the symposium participants.

The study presents a comparative investigation of the yield of gaseous products released during the pyrolysis of a tableted sample of lignite microparticles under the influence of pulsed-periodic laser radiation (6 Hz, 1064 nm, 0.2-2 J/cm²) with nanosecond (12 ns) and microsecond (120 μs) pulse durations. The laser pyrolysis of the coal samples was conducted in an argon atmosphere, with the gaseous products analysed using mass spectrometry. The gaseous pyrolysis products under microsecond pulses contained H₂, CH₄, H₂O, CO, and CO₂, while under nanosecond pulses, H₂, CH₄, C₂H₂, CO, and CO₂ were detected. The yield of gaseous products and the proportion of combustible gases per unit laser pulse energy density were higher for nanosecond laser irradiation. The mass of ablation products from the tableted coal microparticle sample under nanosecond pulses of the same energy density was greater than under microsecond pulses. The observed results are attributed to optical breakdown induced by high-intensity nanosecond pulses, leading to the increased formation of gaseous products and the generation of a stronger shock wave, causing ejection of particles from the tableted sample volume and rapid sample destruction.

A detailed study of high-temperature solid-phase transformations occurring in dispersed microspheres smaller than 10 mm in size (d_m = 3 mm and d₉₉ = 10 mm) belonging to the suspended matter (PM₁₀) of fly ash from the combustion of hard coal from the Ekibastuz and Kuznetsk coal basins has been carried out within the synthesis of glass-ceramics materials. It has been established for PM₁₀ microspheres of macrocomponent composition SiO₂-Al₂O₃-FeO isolated as narrow fractions from fly ash from the combustion of Ekibastuz coal that there is an increase in the content of mullite phase (from 17 to 31 wt%), cristobalite phase is formed (up to 29 wt%); the content of glass phase decreases from 65 to 25 wt%. In the samples of narrow fractions of PM10 microspheres from fly ashes from Kuznetsk coal combustion, crystallisation of the glass phase at 1100 °C leads to a noticeable increase in the concentration of mullite phase (from 3 to 17 wt%), the formation of cristobalite and anorthite phases (3 and 6 wt%, respectively); the amount of glass phase decreases from 93 to 70 wt%. A well-consolidated composite with low porosity (0.4 %), insignificant water absorption (0.2 %), and high strength (56 MPa) was obtained using the direct sintering method based on dispersed microspheres of PM₁₀ fly ash from the combustion of Kuznetsk coal. On the basis of dispersed microspheres of PM₁₀ fly ash from the combustion of Ekibastuz coal, high-porous (open porosity 44-52 %) composites with the homogeneous microporous structure, strength 20-36 MPa, liquid permeability up to 478 L/(m2⋅h⋅bar) and the dispersed microimpurities retention ratio of 0.98-0.99 were obtained. The acid resistance of the obtained glass-ceramic materials is 97-100 %.

The results of laboratory coking are presented for GZh, Zh rank coal (two concentrates from different manufacturers), KZh + Zh, OS rank coal (two concentrates from different manufacturers) in the experimental furnace with 4 kg load, and the studies of resulting coke. The structural strength (S_s) of coke samples was determined according to GOST 9521-2017. Samples were studied by X-ray diffraction analysis, and the sizes of molecularly oriented domains in the coke were determined: domain height (L_c), domain length (L_a), interplanar distance (d₀₀₂), and the number of lamellas (N) in the domain package. The relationship between the structural strength of coke and the chemical-petrographic parameters of coal was studied (the yield of volatile substances per dry state, vitrinite reflectance index, the sum of lean components, the thickness of plastic layer). It has been determined that the structural strength of coke has a quadratic dependence with respect to the chemical-petrographic parameters of coal. According to the experimental results, it is demonstrated that for coke obtained from the OS rank coal, the 0.4 nm difference in L_c and 0.3 nm difference in L_a correspond to a 50 % change in the structural strength of coke. For coke obtained from the Zh rank coal, the 0.28 nm difference in L_c and 0.46 nm in L_a corresponds to a 23 % change in the structural strength of coke. It is concluded that the L_c and L_a indicators make it possible to differentiate the quality of coke by structural strength, unlike for the chemical-petrographic indicators of coal. The general trend of changes in the L_c and L_a domain sizes depending on the structural strength of coke and the stage of coal metamorphism in the sequence GZh, Zh, KZh + Zh, OS is given.

The sorption of sodium, silver, magnesium, calcium, copper, lead and iron cations on the sulphocationite obtained by sulphonation of non-coking long-flame coal of the early stage of metamorphism from the Zadubrovsky open-cast coal mine in the Kemerovo Region was studied. The work primarily focuses on the selective sorption of heavy metal cations (Pb²⁺, Mn²⁺, Ni²⁺, Fe³⁺), which pose a special danger to water resources and human life. The sulphocationite under investigation was obtained by treating the coal with concentrated sulphuric acid and oleum. The dynamic ion exchange capacity of the sulphocationite by strongly acidic groups is 1.4 mg-eq per 1 g of the H-form of dry sulphonic coal (0.7 g-eq/dm³). The equilibrium of cation exchange of protons in SO₃H groups of sulphocationite with Na⁺, Ag⁺, Ca²⁺, Cu²⁺, Mg²⁺, Pb²⁺, Fe³⁺ cations from aqueous solutions at 298 K was studied using the dynamic method. It has been shown that the logarithms of the corrected selectivity coefficients of binary cation exchanges Cat/Н (Cat = Na⁺, Ag⁺, Mg²⁺, Ca²⁺, Cu²⁺, Pb²⁺, Mn²⁺, Ni²⁺, Fe³⁺) depend linearly on the equivalent fraction of cations in the sulphocationite based on long-flame coal. The slopes of the straight lines are associated with the energy inequality of the exchange sites, which make an additive contribution to the Gibbs energy of the system when the counterionic composition of the sulphocationite changes. The studied sulphocationite has unique properties: high capacity and selectivity of metal cation sorption from aqueous solutions. The sorption selectivity of heavy metal cations and the factors of metal/proton separation between the solution and sulphocationite phases increase sharply as the concentration of cations in water decreases. The revealed trend increases in the sequence of heavy metal cations Mn²⁺ < Ni²⁺ < Cu²⁺ < Fe³⁺ < Pb²⁺. The results obtained in the work are promising for the advance in the methodology of deep demineralisation of water using the ion-exchange sorption of metal cations by the sulphocationite based on long-flame coal.

The Pd/N-C catalysts based on the carbon support Sibunite modified by the introduction of nitrogen by the treatment in NO under static reactor conditions were developed. It has been established that at a temperature up to 120 oC the conversion of formic acid is higher over the system Pd/N-C in comparison with the unmodified Pd/C catalyst. X-Ray photoelectron spectroscopy was used to identify the states of nitrogen and palladium in the resulting systems. Transmission electron microscopy was used to study the particle formation trends in the Pd/C and Pd/N-C catalysts, as well as their thermal stability.

A systematic study employing scanning electron microscopy and energy-dispersive X-ray spectroscopy (SEM-EDS) of ferrospheres isolated from the fly ash formed in the combustion of pulverised coal of the Kuznetsk Basin allowed us to determine the glass phase composition. The groups of globules have been identified for which the gross composition of polished sections exhibits a linear correlation between the content of glass-forming silicon and calcium oxides. Heterogeneity of the glass phase of the studied ferrospheres in composition and the number of its components was established. It is shown that iron is mainly found in the crystallites of iron-containing phases, and silicon is in the glass phase. The remaining elements are distributed between these phases. It is shown that ferrospheres contain microglobules of varying compositions, with sizes of less than 1 mm, localized in the amorphous glass phase. Their presence determines the chemical heterogeneity of the glass phase. The composition of microglobules, like the composition of ferrospheres as a whole, is determined by the mineral components of the original coal. The precursor for the formation of the glass phase of ferrospheres are aluminosilicates of original coal.

The possibility to generate acetylene by pyrolysis in hydrogen plasma was determined using thermodynamic calculations taking into account the elemental composition, temperature range, and the C/H ratio for coal samples from six open-cut mines of the coal deposits of Eastern Siberia: the Mugunsky production site of Tulunugol (ZBR coal rank, the Irkutsk Region), Chadan (GZh coal rank, the Republic of Tyva), Zalushansky (D coal rank, the Trans-Baikal Territory), Irbeysky (2BR coal rank, the Krasnoyarsk Territory), Cheremkhovugol (G coal rank, the Irkutsk Region), Kaakhem (G coal rank, the Republic of Tyva). Results of thermodynamic calculations for the listed coal samples demonstrate the possibility to obtain acetylene from all the six coal ranks under consideration. These results can be used to develop the technology for obtaining acetylene and other compounds by the hydrogen-plasma pyrolysis of coals from the deposits of Eastern Siberia.

The dependence of the indicators of thermal decomposition of coal from the Kuzbass and Pechora basins on coal moisture was studied when determining the liability of coal to spontaneous combustion by thermogravimetric analysis. The rates of mass change were calculated, and characteristic temperature points were determined (the onset of mass increase, and the maximum rate of mass change) by heating the coal samples within temperature ranges 120-300 and 300-900 °C. It has been determined that the rate of mass gain within the range of 120-300 °C is 10 times higher for the coals of the Pechora coal basin, prone to spontaneous combustion, while within the range of 300-900 °C it is independent of the tendency of coals to spontaneous combustion. It is shown that with an increase in the moisture content in coal, the rate of thermal decomposition of coal increases with an increase in moisture content within the temperature range of 25-200 °C. Moisture content of coal was not detected to affect the parameters (the temperature points of oxidation onset and mass gain) characterising coal oxidation reaction in the studies by thermogravimetric analysis.

As a result of studying the phase composition of Ni-Pt nanoalloy particles using X-ray diffraction (XRD) analysis, it has been established that during the synthesis of Ni-Pt nanoalloy particles by co-reduction of the aqueous metal precursor solutions (Ni²⁺ and [PtCl₆]^2-) with an alkaline hydrazine hydrate solution, the formation of fcc-type Ni-Pt solid solution particles occurs, with an average Ni content of 13 at%. These particles have ellipsoid shape with the equatorial and lateral size 6-13 and 10-28 nm, respectively. By comparing the XRD results with data obtained from high-resolution transmission electron microscopy (HRTEM) and small-angle X-ray scattering (SAXS), it has been shown that, in addition to the aforementioned Ni-Pt solid solution particles, the synthesised samples contain ultrafine Ni-rich particles: the phases of Ni-Pt intermetallides and the fcc-phase of individual Ni. As a result of heating the sample with total nickel content 20 at% in high vacuum to a temperature of 390 °C, the phase transformation takes place, leading to the formation of fcc-type Ni-Pt solid solution particles with Ni content 23 at% and average size ≈26 nm, as well as the particles of practically pure platinum with the average size ≈55 nm.

The problem related to processing and disposal of ash and slag waste from thermal power facilities has not been solved in Russia as a whole, and particularly in Kuzbass. In the present work, we studied ash and slag (slag, fly ash from Kemerovo and Belovo heat plants, and Kemerovo power plant) and related wastes (cake and ore from the enrichment plant) from the enterprises of Kuzbass using physicochemical methods to assess the optimal ways of their processing. X-Ray diffraction analysis has shown the presence of quartz in all the studied wastes, carbon-like phases in rocks and cake, and vitreous phases in all slags and the vast majority of fly ash samples. The materials were analysed by atomic emission spectroscopy with inductively coupled plasma after autoclave preparation of the sample with a mixture of nitric and hydrochloric acids. X-Ray fluorescence analysis was performed for rocks and cake. Element content in samples, assessed from atomic emission analysis data, correlates with the data of X-ray fluorescence analysis. Fly ash, ash and slag wastes differ from each other in composition: fly ash is characterised by lower magnesium and iron content. It is shown that glass formation in ash and slag at high combustion temperatures complicates the acid extraction of elements. The method of acid leaching with nitric acid followed by precipitation with a solution of ammonia and oxalic acid was tested. Rare earth elements are observed to concentrate in the fraction of insoluble hydroxides, where aluminium prevails as the major element; in particular, europium is concentrated up to 144 g/t. Low calcium content, high silicon and aluminium content allowed us to propose manufacture of silicate products with the possibility of isolating rare and rare earth elements as the main way of processing the wastes from the enterprises of fuel and energy complex of the Kemerovo Region (Kuzbass).

The work is focused on the preparation of zinc ferrite and study of its catalytic activity in the phenol ozonolysis reaction in an aqueous medium. Zinc ferrite was synthesised by co- precipitation of the hydroxides with ammonia solution, followed by hydrothermal treatment of the precipitate at a temperature of 160 °C. The product was characterized by X-ray diffraction and infrared spectroscopy. The catalytic activity of zinc ferrite in phenol ozonolysis was studied. It has been determined by UV-Vis spectroscopy that the products of phenol oxidation are cis,cis-muconic acid (absorption in the region of 300-400 nm) and 1,4-benzoquinone (absorption band at 237 nm). It is shown that the addition of zinc ferrite not only accelerates phenol ozonolysis but also causes deeper oxidation; 1,4-benzoquinone is not formed if the catalyst is absent. The data obtained can be used to develop new water purification technologies based on a combination of ozonation and heterogeneous catalysis.

The results of an experimental study of high-temperature plasma gasification of mixed organic fuel based on sawdust and coal washing waste (hereinafter referred to as coal) are presented. The relevance of the work is due to the need to develop effective and environmentally friendly methods for processing renewable raw materials in the context of increasing energy consumption and tightening environmental standards. Gasification of individual components (sawdust, coal), their mechanical mixtures and composite materials obtained by their joint activation milling in various ratios was studied. The experiments were conducted in a plasma-thermal unit with a capacity of 20 kg/h with an arc plasma torch (50 kW) at temperatures of 1200-1600 °C. The experiments showed that the maximum concentrations of the target components of the synthesis gas were achieved during gasification of a mixture containing 66 % sawdust and 33 % coal. In this version, the hydrogen content in the gasification products reached 9.91 vol%, and carbon monoxide - 28.04 vol%, which indicates a high efficiency of processing such a fuel composition. Analysis of the gas evolution dynamics revealed that in comparison with mechanical mixtures, the composite samples obtained by the joint activation milling provide a more stable and uniform yield of synthesis gas throughout the gasification process, which is important for the practical application of the technology. The studies have shown that the combined processing of biomass and coal in the form of composite materials allows optimising the gasification process, ensuring uniform gas emission and reducing harmful emissions. The results obtained are of practical importance for the development of energy-efficient and environmentally friendly technologies for processing organic waste.

Hollow aluminosilicate microspheres (cenospheres) of stabilised composition (glass phase - 95.4 wt%; (SiO₂/Al₂O₃)_glass - 3.1) isolated from coal fly ashes from coal combustion were used to prepare composite sorbents containing a sorption-active component based on zirconosilicates of framework structure. The synthesis products were characterised by X-ray diffraction analysis, scanning electron microscopy with energy-dispersive X-ray spectroscopy, and their sorption properties for Cs⁺, Pb²⁺ and Cd²⁺ cations were studied. The zirconosilicate material shows a high distribution coefficient in the process of sorption of Cs⁺, Pb²⁺ and Cd²⁺ from aqueous solutions (10³-10⁵ mL/g). For Pb²⁺ as an example, it is shown that as a result of high-temperature phase transformation of the Pb²⁺-form of zirconosilicate, Pb²⁺ cations are stabilised in the crystalline phase of lead zirconate PbZrO₃. The possibility to use spark plasma sintering for obtaining mineral-like ceramics based on zirconosilicate sorbent for immobilisation of radionuclide Cs-137 has been investigated. For ceramics sintered at different temperatures (800-1000 °C) the cesium leaching rate was studied, which is a criterion of hydrolytic stability of radioactive ceramics intended for disposal in rocks. The obtained values of leaching rate (~10^-5 g/(cm²⋅day)) meet the requirements of Federal Norms and Rules in the area of atomic energy use NP-019-2000 “Collection, processing, storage and conditioning of liquid radioactive wastes. Safety requirements”.

Modes of modification of carbon material obtained from wood raw materials are described in order to improve the electric capacitance characteristics for subsequent application as an electrode material in supercapacitors. The effect of two modification methods is considered: treatment with hydrogen at 1000 °C, treatment with a concentrated solution of hydrogen peroxide (37 wt%) at 60 °C. It is revealed that the greatest improvement in the functional properties of the material occurs when it is treated with hydrogen peroxide. Analyzing the sorbometry data, it was found that the specific surface area of the sample modified in this way increases by 20 % due to the formation of micropores. In this case, according to IR spectroscopy data, electrochemically active carbonyl groups are formed in the sample. Testing of the obtained electrode material in a model electrochemical cell simulating supercapacitor operation revealed an increase in its electrical capacity by 60 % relative to the initial sample.

An integrated method of mining quarry reclamation and landscaping is presented. The essence of the method is in making a protective layer of gel-forming composition, based on polyvinyl alcohol (PVA) and IKhN-PRO composition, including borax, on the surface of solid toxic rock. A fertile ground containing plant seeds is applied onto the surface of the protective layer; its surface is treated with a solution of PVA mixture and carboxymethylated starch (CMS). After the freezing-thawing cycle, soil-structuring cryogel is formed, which retains moisture, heat and makes comfortable conditions for plants. The rheological properties of the gel-forming composition were investigated; the time of gel formation at a temperature of 20 and 10 °C was determined to be 200 and 150 seconds, respectively. The rheological characteristics of the solutions of PVA and CMS mixture were studied. It is shown that with an increase in the polymer concentration in the mixture the viscosity increases. Dry films obtained on the basis of a mixture of PVA, CMS and cryogels swell in water. Phytotoxicity of the method was studied for coal samples. The biometric data of plants have shown that the productivity of plant biocenosis in experimental samples is much higher than in control samples.

A new oil-in-water microemulsion composition has been proposed, incorporating a suite of multifunctional chemical additives (surfactants, improver additives) produced and marketed in Russia. The composition is intended for use as a hydraulic fluid for mechanised mine supports. The physicochemical properties of the developed concentrate and the well-known SOLCENIC GM 20 microemulsion concentrate (Fuchs, Germany) are close to each other. The developed microemulsion concentrate is recommended as a replacement for the foreign-made product.

During the operation of ash dumps, process water at the base of man-made massifs forms a man-made aquifer characterised by high mineralisation, hydrocarbonate-calcium-sodium composition, and a highly alkaline environment. Based on the presented studies of the aquatic environment and previously obtained data on the material composition of the solid phase of man-made deposits, the influence of the aggressive composition of waters in the man-made aquifer on the qualitative composition of ash and slag has been analysed. It is revealed that the ongoing disintegration of carbonates and aluminosilicates in the lower horizon of ash and slag massifs lead to the release of a wide range of hazardous substances. Technogenic processes have a significant impact on the qualitative composition of technogenic filtrate and the migration activity of water-soluble ingredients, which can significantly affect the state of the environment and require systematic environmental monitoring.

The use of high-calcium fly ash (HCFA) as an expanding component of cements contributes to an increase in the level of their utilisation and improvement of binding properties. The influence of HCFA fractions of different size and composition on the expanding effect of binders based on them is studied in the work. The binders based on 100 % of three industrial fractions of high-calcium fly ash of different dispersion and composition, sampled from the 1^st, 2^nd and 4^th fields of the Krasnoyarsk TPP-2 electrostatic precipitators, were studied; the expanding effect of binders based on these fractions was determined with respect to Portland cement (PC) grade CEM I 42.5N. It was determined that an increase in the volume of hardening specimens is 6-19 and 6-42 % after hardening for 5 and 120 days, respectively. An increase in the volume of specimens correlates with the content of CaO and MgO oxide phases in the initial HCFA fractions and is accompanied by a decrease in the average density and compressive strength. The specimens of cement-fly ash compositions with the content of 50 % PC and 50 % HCFA, including a mixture of different fractions of FA, were studied. The positive effect of HCFA fractions on the properties of composite cement, including the regulation of the expansion effect and an increase in compressive strength, was determined.

The procedure for the quantitative determination of F, P, S, V, Cr, Co, Ni, Cu, Zn, As, Pb, Th, and U in the samples of coal and in soil samples containing coal is described. X-Ray fluorescence (XRF) analysis was carried out using wavelength-dispersive X-ray fluorescence spectrometer S8 TIGER (Bruker, Germany). Measurements were carried out in the vacuum mode. The dried samples were prepared in the form of pressed tablets. To obtain calibration characteristics and carry out metrological studies, a set of certified reference materials (CRMs) of shale, coal ash, sediments and soils of different chemical composition was chosen, and mixtures with different CRMs powders and graphite content were prepared. The ratio of CRMs to graphite was determined according to the data on total carbon content in the objects under investigation, and the data on the ash content of coal. To account for mutual influences of the elements, the a-correction method was used, in most cases introducing the fluorescence intensities of elements present in the samples (carbon, etc.) as influencing factors. The calculated values of the detection limits for the elements under determination vary from 0.6 to 20 mg/kg. The accuracy of XRF analysis results was controlled using CRMs of shale (SGR1 and SDC1), anomalous silt (SGH5) and black soil (SP1), as well as the mixtures of SGHM3/graphite (1 : 4) and DVT/graphite (1 : 3). It has been determined with t-test that the results of XRF analysis do not contain significant systematic errors. The procedure for X-ray fluorescence determination of F, P, S, V, Cr, Co, Ni, Cu, Zn, As, Pb, Th and U was used to study the distribution of elements in the samples of coal fractions from the deposits of the Irkutsk Region and in the samples of soils containing these fractions, which were collected in the residential area of the Oktyabrsky district of the city of Irkutsk during summer 2024. Based on XRF data, the conclusion concerning the effect of long-term coal presence in soils on their elemental composition is made.

The results of experiments on the direct oxidation of benzene to phenol using oxygen and air in a barrier discharge under the conditions of efficient removal of reaction products from the reaction zone are presented. In the case of benzene oxidation with oxygen, phenol content in the products reaches ~73 wt%, while arenediols are formed in insignificant amounts (~8 wt% as a total, mainly hydroquinone). The oxidation of benzene with air leads to an increase in the phenol content in the products to ~77 wt% and a decrease in the content of diatomic phenols to ~3 wt%. The conversion of benzene per single pass of the vapour-gas mixture through the reactor reached 0.5 wt% in oxygen and 0.4 wt% in air. The direct oxidation of benzene to phenol with air is accompanied by the formation of a precipitate. Its structure has been studied, and the mechanism of its formation has been discussed. It has been shown that the formation of the precipitate during benzene treatment with air is caused by reactions involving excited nitrogen molecules. The main stages of the mechanism of oxidation are considered in detail, and the results of calculations of electron energy losses in electron-molecular reactions occurring at the discharge initiation stage in the barrier discharge are presented. These calculations allow estimating their contribution to the mechanism of formation of intermediate active particles and stable molecules, as well as the routes of the benzene oxidation process in the barrier discharge plasma. It has been demonstrated that phenol formation occurs as a result of direct interaction between the benzene molecule and atomic oxygen. It has been shown that phenol formation occurs as a result of the direct interaction of the benzene molecule with atomic oxygen. It is demonstrated that benzene oxidation in the barrier discharge surpasses some thermocatalytic methods in terms of reaction rate and exhibits comparable results in terms of phenol formation selectivity.

The effect of low-temperature Ni-Ti eutectics on the mechanochemical in situ synthesis of titanium carbide in a nickel matrix has been studied by X-ray diffraction methods and X-ray spectral microanalysis. When comparing the systems containing 50 wt% Ti-(Ti-C) and 50 wt% Ni-(Ti-C), it has been determined that in the first case the induction period of reaction is 4 min, and in the second case the synthesis proceeds in a mechanically stimulated reaction mode with an induction period of 110 s and is fully completed by 120 s. By the time of reaction completion (120 s), a significant amount of TiC_x (up to 38 wt%) with higher carbon content (C/Ti = 0.83) is detected in the reaction mixture with 50 wt% Ni, and the formed crystallites are larger (~30 nm) than in the mixture 50 wt% Ti + (Ti + C), which justifiably suggests a liquid-phase synthesis mechanism. In the reaction mixture with 50 wt% Ti, by 4 min of mechanical activation, up to 42 wt% TiC_x with crystallite size ~9 nm is formed. In the system 50 wt% Ni-(Ti-C), the dispersed hardening of nickel with titanium carbide is enhanced by solid-solution hardening, as evidenced by the formation of Ni(Ti) solid solution within the same synthesis time intervals (120 s). Shortening of the induction period can significantly reduce the contamination of synthesis products with the material of grinding media and drum walls.