Abstract (English):
The main objective of this book is to acquaint the reader with the main modern problems of the multisensor data analysis and opportunities of the hyperspectral shooting being carried out in the wide range of wavelengths from ultraviolet to the infrared range, visualization of the fast combustion processes of flame propagation and flame acceleration, the limit phenomena at flame ignition and propagation. The book can be useful to students of the high courses and scientists dealing with problems of optical spectroscopy, vizualisation, digital recognizing images and gaseous combustion. The main goal of this book is to bring to the attention of the reader the main modern problems of multisensory data analysis and the possibilities of hyperspectral imaging, carried out in a broad wave-length range from ultraviolet to infrared by methods of visualizing fast combustion processes, propagation and flames acceleration, and limiting phenomena during ignition and flame propagation. The book can be useful for students of higher courses and experimental scientists dealing with problems of optical spectroscopy, visualization, pattern recognition and gas combustion.

Keywords:
Remote measurements, optoelectronic methods, multisensor data analysis, hyper spectral shooting, ramjet engine, Catalytic Stabilization

Copper nanopowders are obtained by the method of hydrogen reduction (chemical-metallurgical method) and thermal decomposition of copper citrate and formate. It was shown that copper nanopowder synthesized from copper citrate is not pyrophoric. Combustion of this copper nanopowder can be initiated by an external source, with the combustion wave velocity being 1.3 ± 0.3 mm/s. The nanopowder has a ~ 4 times larger specific surface area than the nanopowder obtained by the chemical-metallurgical method. It practically does not contain oxides and is stable in atmospheric air. Copper nanopowder obtained by the chemical-metallurgical method is pyrophoric and therefore requires passivation, but its passivation leads to the formation of noticeable amounts of copper oxides. The burning rates of passivated and non-passivated copper nanopowder obtained by the chemical-metallurgical method are the same. Tungsten nanopowders are synthesized by reduction of tungsten trioxide with hydrogen (chemical metallurgy method) at 440÷640 °C from samples with different specific surface. It is shown that the W nanopowder synthesized at 640 °C for all three precursors used is non-pyrophoric -W. Its combustion can be initiated by an external source. Combustion develops in a spatially non-uniform regime. Nanopowder synthesized at 480 0C from tungsten oxide grades 1 and 2 is a mixture of -W, -W и WO2.9. This powder is pyrophoric. It was found that the passivated W nanopowder synthesized at 480 °C from grade 3 tungsten oxide is 480 0C are W with traces of WO3 and WO2.9. temperature range of synthesis W, obtained in the work is very narrow: 470÷490 0C. The specific surface area of -W nanopowders is 10 ± 2 m2/g. It is 18 ± 1 m2/g for the -W mixture with traces of WO3 and WO2.9. The dynamics of temperature fields during the ignition and combustion of tungsten nanopowders obtained at different temperatures has been studied. Preliminary experimental studies of the combustion features of compact samples made of non-passivated iron nanopowders and the effect of the porosity of these compact samples on the dynamics of their heating in air have been carried out. The aim was to establish the temperature range at which it is possible to safely carry out technological operations with compact samples of non-passivated iron nanopowders. Key words: combustion mode, nanopowders, pyrophoricity, compacting, infrared video camera Metal nanopowders are pyrophoric, i.e. are capable of spontaneously igniting on contact with air due to their high chemical activity and large specific surface area. There are two main ways to ensure fire and explosion safety of technological processes: passive engineering, based on warning systems of undesirable changes in the process, and scientific and technological, involving such a change in the technological process or materials used in the process, which leads to the fact that the technological the process becomes less dangerous or safer. In order to make the process of further processing of nanopowders into products safe, they are passivated. Passivation consists in creating a thin protective film on the surface of nanoparticles, which prevents spontaneous combustion of metal nanopowders. Passivation lasts tens of hours, which is a limiting factor in increasing the production of nanopowders. We have previously formulated a model of the passivation of a pyrophoric nanopowder layer and analyzed it by analytical and numerical methods [1-3]. Assuming the limiting role of oxidant diffusion in the mechanism of propagation of the passivation wave, the dependence of the temperature in the heat release zone on the governing parameters is obtained. It is shown that for the maximum temperature in the nanopowder layer there is an intermediate asymptotic behavior when the temperature does not change with time. An approximate formula for calculating the minimum time of full passivation for backfill of arbitrary thickness is obtained on the basis of experimental data for a specific backfill. The applicability of theoretical approaches of the classical macroscopic theory of thermal explosion to explain the phenomena of ignition in macroscopic objects consisting of iron and nickel nanoparticles is shown. The results of recent work with the participation of the authors of this book are demonstrated below. Along with the establishment of the features of the combustion of copper and tungsten nanopowders, preliminary experimental studies of the features of the combustion of compact samples of non-passivated iron nanopowders and the effect of the porosity of these compact samples on the dynamics of their heating in air are described. The goal is to develop new highly efficient methods for producing compact products from nanopowders, which make it possible to provide the required level of fire and explosion safety both in the processing of nanopowders and products made from them. The research described in Chapter 8 was supported by a grant from the Russian Science Foundation (project No. 16-13-00013). § 1. Combustion of copper nanopowders Copper nanoparticles have attracted considerable attention in recent years due to their wide possible application in photochemical catalysis, in bio- and electrochemical sensors, photovoltaic energy converters, and medicine [4-11]. The synthesis of copper nanoparticles is carried out by methods of chemical reduction [8], thermal decomposition of precursors [12], explosion of thin wires, etc. [13-18]. Copper nanoparticles can be pyrophoric, therefore, in order to make possible subsequent processing of nanopowders in atmospheric air, they must either be stored under an inert liquid or protected. Protection (passivation) means obtaining a thin oxide film on the surface of nanoparticles, which prevents the oxidation of nanoparticles and ensures the preservation of their unique properties [19] during or after synthesis. The purpose of this section is to identify the thermal regimes and dynamics of ignition and combustion of copper nanopowders obtained by the chemical-metallurgical method and the method of thermal decomposition of copper salts, to establish the conditions for their passivation to prevent ignition and subsequent oxidation. A number of characteristics of synthesized copper nanopowders have been determined using X-ray phase analysis, BET and scanning electron microscopy methods. For experimental studies, we used copper nanopowders obtained both by the chemical-metallurgical method and by thermal decomposition of copper citrate and formate salts. The main stages of the synthesis by the chemical-metallurgical method are the preparation of a precipitate of metal hydroxide, its drying, reduction and passivation. The synthesis of copper hydroxide was carried out by heterophase interaction of CuCl2 with an alkali solution. After precipitation of hydroxide, it was washed with water in a Buchner funnel to pH = 7 and dried in air until dusting. A quartz boat with copper hydroxide powder was installed inside a quartz reactor and placed in an oven heated to 80 °C for 1 h while blowing hydrogen through the reactor. Then the reactor with the boat was removed from the furnace and cooled to 20 °C in an argon flow through the reactor. Then the reactor was placed on a subject table for video recording, and a quartz boat with copper nanopowder was removed from the reactor and placed next to it. Then the boat with copper nanopowder and the reactor were either blown with air using a fan, or the air fan was turned off. In some experiments, copper nanopowder was passivated in an argon flow containing 0.6% oxygen for 30 min and only then was removed from the reactor. Thermal decomposition of copper citrate Cu3 (C6H5O7) 2 (at 350 °C) and copper formate (C2H2CuO4) (at 250 °C) was carried out in the same reactor, in vacuum with continuous pumping out of the gas released during the decomposition of salts using a forevacuum (2NVR-5D ) and diffusion (H1) pumps. When the salt was heated, an increase in pressure was first recorded from 10-4 Torr to> 10-1 Torr. The decomposition was considered complete when the pressure in the reactor became less than 10-2 Torr. Then the reactor was removed from the furnace and cooled with continuous evacuation of gas. After cooling to 20 °C, argon was admitted to the reactor to atmospheric pressure, and only then the quartz boat with copper nanopowder was removed from the reactor and placed on a subject table for video recording. The process of removing the boat and placing it on the table took about 5 s. Casio Exilim F1 PRO high-speed color video camera (60-1200 frames per second) and Flir 60 infrared camera (shooting speed 60 frames/s, resolution 320x240 pix, sensitivity interval 8-14 microns) were used to study the ignition and combustion modes of copper nanopowder. The phase composition of the obtained samples was studied using a DRON 3M X-ray diffractometer with a coordinate-sensitive sensor. The specific surface area was measured using a Sorbi-M analyzer by the BET method. The microstructure of the powders was studied using an ultrahigh-resolution scanning electron microscope Zeiss Ultra Plus (Germany) equipped with an INCA 350 Oxford Instruments X-ray microanalyzer. Combustion in air of a copper nanopowder obtained by the chemical-metallurgical method by holding it in a furnace for 1 h at 80 °C and blowing hydrogen through a reactor (a 2-millimeter-thick sample) is shown in Fig. 1a. Self-ignition, leading to combustion of the sample, occurs only when it is blown with air. Spontaneous combustion is not observed without blowing. The propagation velocity of the combustion front over the sample surface, estimated as the average velocity over three points selected at different parts of the front, is 0.3 ± 0.02 mm/s. The sequential frames of initiated combustion in air of copper nanopowder (2 mm layer thickness) obtained under the same conditions by the chemical-metallurgical method in the absence of blowing are shown in fig. 1b. Filming was carried out with a Flir 60 infrared camera. Fig. 1. Combustion in a stream of air of copper nanopowder obtained a) chemical-metallurgical method (sample of 2 mm thickness). At the bottom of each frame on the right is the time in seconds after the boat with the nanopowder was removed from the reactor. Initial powder temperature is 20 °C. The shooting speed is 60 frames per second. b) A sequence of frames of infrared video recording of the combustion of copper nanopowder (2 mm layer thickness) obtained by the method of chemical metallurgy. There is no air flow. The initial temperature of the powder is 20 °C. The shooting speed is 60 frames per second. The left frame shows the temperature distribution on the sample surface at the moment of maximum self-heating. The three right frames show the initiation and combustion of the same sample of copper nanopowder with a heated wire (the front propagates from left to right). The time in minutes is indicated at the bottom of each frame on the right: seconds after being removed from the reactor. In case of visual analysis of infrared video data, one should take into account the peculiarities of image processing with the Flir 60 infrared camera: the area with the maximum temperature value at a given time has the same brightness for all frames. The real values of the maximum and minimum temperatures at a given time are shown near the left border of each frame. The larger cross on each frame indicates the selected point at which the temperature is measure. The smaller cross with a red flag automatically points to the point with the maximum temperature in the frame, and the smaller cross with a blue flag to the point with the minimum temperature in the frame. The left frame in Fig. 1b shows the temperature distribution over the sample surface at the moment of maximum self-heating, which is 88 °C. This local heating in the center of the sample did not lead to the propagation of the reaction front, but after cooling, it turned out to be possible to initiate combustion with a heated wire of the same sample of copper nanopowder in air (the next three frames in Fig.1b). The maximum combustion temperature reaches 407 °C, and the reaction front velocity is 0.3 ± 0.04 mm/s and is consistent with the experiment shown in Fig. 1a. Therefore, if the sample is blown, then the air freely reaches the surface of the powder, and self-ignition occurs. In the absence of blowing, residual argon flows out of the reactor near the boat and makes it difficult to supply oxygen from the atmosphere to the sample. Therefore, self-ignition is absent. Since such a slight change in the experimental conditions leads to qualitative changes in the modes of interaction of the copper nanopowder with air, this indicates the high sensitivity of the copper nanopowder to the conditions of the experiments. Measurements of the specific surface area of a non-passivated nanopowder (obtained without blowing) and passivated for 30 min in an argon flow containing 0.6% mass of oxygen at 20 °C showed that they are 13 ± 2 m2/g and 10 ± 2 m2/g, respectively. The value of the average diameter of nanoparticles can be estimated by the formula d = 6 / ( s), where s is the specific surface area, gcm is the copper density. For non-passivated and passivated nanopowders, calculation by the formula gives the value of the average diameter of copper nanoparticles d = 47 nm and d = 61 nm, respectively. Consequently, passivation does not lead to a qualitative change in the specific surface area of a copper nanopowder and nanoparticle sizes. The modes of combustion of copper nanopowders obtained by decomposition of salts is demonstrated in fig. 2. Hot-wire-initiated combustion of copper nanopowder (2-mm layer thickness) in air (without blowing) obtained from copper citrate at 350 °C is shown in fig. 2a. The speed of the combustion front of copper nanopowder obtained from copper citrate is 1.3 ± 0.3 mm/s. It turned out that only the surface layer is oxidized in the combustion wave, while the inner part of the sample remains combustible. Indeed, if the continuity of the oxide layer is violated, the powder inside ignites (see frames 182, 259 s). The specific surface of the nanopowder after synthesis, determined by the BET method, is 45 ± 5 m2/g, and the average diameter of copper nanoparticles is d = 14.6 nm. Fig 2. a) Sequences of video footage of initiated combustion in air of copper nanopowder (2 mm layer thickness) obtained from copper citrate at 350 °C. At the bottom of each frame on the right is the time in seconds after the boat with the powder was removed from the reactor. b) Sequences of frames of infrared video recording of initiated combustion in air of copper nanopowder (2 mm layer thickness) obtained from copper citrate at 350 °C. At the bottom of each frame on the right is the time in minutes - seconds after the boat with the powder was removed from the reactor. Despite such a high specific surface area, we were unable to obtain self-ignition of the sample, even if the residual pressure in the reactor after the decomposition of copper citrate was 5.10-5 Torr. This is inconsistent with the results of [20], in which the copper powder obtained by the decomposition of copper citrate ignited spontaneously in air at a pressure in the reactor after the completion of decomposition equal to 10-3 Torr. Thus, the regimes of combustion of a copper nanopowder layer could be realized only when it is initiated by a heated wire. The frames of infrared video recording of copper nanopowder (two-millimeter layer thickness), initiated by a heated wire combustion in air, obtained from copper citrate at 350 °C in fig. 2b. It can be seen that the combustion front propagates over the sample surface initially, and the bulk of the nanopowder continues to react when the surface combustion front has already passed. This is evidenced by the long (tens of seconds) retention of a high temperature in the region of the sample where the combustion front passed, and the movement of the temperature maximum (the location of the smaller cross with a red flag) in the opposite direction: from the left end of the sample to the central part (see frames 2.28, 2.47). The maximum temperature in the combustion front reaches 611 °C. Based on the data obtained (large specific surface area, high velocity and temperature of the combustion front), it could be expected that copper nanopowder synthesized from copper citrate will be pyrophoric. However, copper nanopowder obtained from copper citrate does not self-ignite, i.e. not initially pyrophoric. The stability of this non-pyrophoric nanopowder can be associated with the “poisoning” of copper with CO [21], which is formed during the thermal decomposition of citrate. It should be noted that, during the decomposition of copper formate, along with copper powder, a copper foil is formed on the inner surface of the boat. Copper powder contains relatively large crystallites. In contrast to the methods for producing copper powders described above, self-sustaining combustion was not possible even when it was initiated with a heated wire. The combustion process dies out starting near the spiral. The results obtained allow us to conclude that the thermal decomposition of copper formate is not a promising method for producing copper nanopowder. The photographs of Cu nanopowders synthesized by the chemical-metallurgical method and passivated for 30 min with a mixture of 0.6% air with argon at 20 °C (a) and thermal decomposition of copper citrate (b), obtained by scanning electron microscopy (Zeiss Ultra Plus / INCA 350 Oxford Instruments) are shown in fig. 3a, b. As can be seen from the figure, sample (a) consists of sintered agglomerates. Particles with a size of 100-200 microns and less than 20 microns are present. However, they are all sintered agglomerates of smaller particles. Fig. 3. Microphotographs of copper nanopowders obtained by (a) chemical-metallurgical method (passivation for 30 minutes) and (b) thermal decomposition of copper citrate Sample (b) is uniform in particle size about 10-30 microns. These particles are agglomerates of particles with a size of about 100 nm, located in a matrix, which is visible in the photograph as a "binding glue" between the particles. The hierarchy of the structure is well traced. Particles less than 100 nm in size stick together into structures with a size of 1-2 microns, which in turn form separate agglomerated particles with a size of 10-30 microns (not shown in the figure). On particles less than 100 nm in size, particles of even smaller size (less than 10 nm) are also observed, but it is not entirely clear whether 100 nm particles consist of 10 nm objects, or just 10 nm particles cover 100 nanometer particles. X-ray phase analysis of copper nanopowders obtained by a) chemical-metallurgical method (sample 2 mm thick, passivation for 30 min); b) from copper citrate (circles - Cu, rhombuses - Cu2O, squares - CuO) is shown in Fig. 4. As can be seen from the Figure, even passivated copper nanopowder obtained by chemical metallurgy contains noticeable amounts of Cu2O and CuO. In this case, the nanopowder obtained from copper citrate contains only traces of CuO, i.e. the production of copper nanopowder by the thermal decomposition of salts is more promising since the signal of copper oxides is practically absent. Fig. 4. Data of X-ray phase analysis of copper nanopowders obtained a) from copper citrate, b) by the method of chemical metallurgy (2 mm thick sample, passivation for 30 min). Circles - Cu, rhombuses - Cu2O, squares - CuO. We briefly list the results of this section. Copper nanopowders are obtained by the method of hydrogen reduction (chemical-metallurgical method) and thermal decomposition of copper citrate and formate. It was shown that copper nanopowder synthesized from copper citrate is not pyrophoric. Combustion of this copper nanopowder can be initiated by an external source, with the combustion wave velocity being 1.3 ± 0.3 mm/s. The nanopowder has a ~ 4 times larger specific surface (45 ± 5 m2/g) than the nanopowder obtained by the chemical-metallurgical method, practically does not contain oxides and is stable in atmospheric air. Copper nanopowder obtained by the chemical-metallurgical method is pyrophoric and therefore requires passivation, but its passivation leads to the formation of noticeable amounts of copper oxides. The combustion rates of passivated and non-passivated copper nanopowder obtained by the chemical-metallurgical method are the same and amount to 0.3 ± 0.04 mm/s. The dynamics of temperature fields during the ignition and combustion of copper nanopowders obtained by various methods has been studied. §2. Combustion of tungsten nanopowders Tungsten-based nanomaterials have advantages as electron emitters. Elements of photocopiers, laser printers and air cleaners, chargers, nanodevices with chemical sensors, biomedical sensors, antistatic coatings can be made from nanoscale powders including tungsten. Tungsten-based nanomaterials are used in cathode-ray tubes, displays, X-ray anodes, klystrons, magnetrons for microwave ovens [22]. This section presents the results of studying the temperature regimes of synthesis of tungsten nanopowder with different crystal structures, determining the optimal passivation regimes and studying the regularities of the ignition and combustion of nanopowder obtained under various conditions [23]. The stable crystal structure of tungsten (-W) is face-centered cubic. There is a metastable form of tungsten (-W), which has a cubic crystal structure A-15, containing eight atoms per unit cell [24]. Tungsten (-W) has a giant spin Hall effect, which makes this material very promising in spin electronics. This is a branch of quantum electronics dealing with the study of spin current transfer (spin-polarized transport) in solids, where, along with the charge, the electron spin is an active element for storing and transmitting information, forming integral and functional microcircuits, designing new magneto-optoelectronic devices [25 - 27]. The spin Hall effect is considered as a promising mechanism for generating spin-polarized current, which does not require the use of a magnetic field or ferromagnetic materials [28]. β-W with its giant spin Hall effect, is among the materials with the highest efficiency in converting electric current into spin current, which is accepted as a prototype in the design of spin electronics devices [29, 30]. Although β-W was discovered more than 60 years ago [31], there was no understanding of the mechanism of β-W formation. It has been shown that β-W formation is sensitive to deposition parameters such as inert gas pressure and the presence of oxygen impurities. However, there are no empirical models that could describe the relationship between the β-W formation mechanism and deposition parameters. In particular, the role of oxygen impurity is still being discussed [29, 30], since it is assumed that β-W is a nonstoichiometric oxide with the formula W3O, while it is known that oxygen in β-W films has zero valence, i.e. β-W is an allotrope of α-W [32]. The purpose of this section is to establish the modes of combustion and passivation of tungsten nanopowders, as well as the modes of synthesis of nanopowders by the method of chemical metallurgy [33] in order to determine the temperature ranges of formation of W and β-W. Partial characterization of the synthesized nanopowders W was carried out. In the experiments, we used WO3 samples with different specific surface: 2 m2/g (WO3 (1, ISMAN)), 11 m2/g (WO3 (2)), Novosibirsk, http: // rare metal. ), 0.8 m2/g (WO3 (3)), UK Cat No.B1188). A quartz boat with tungsten trioxide powder WO3 1-3 mm thick was installed inside a cylindrical quartz reactor and placed in a furnace heated to 450 ÷ 650 °C for 2-5 h while blowing hydrogen through the reactor (Fig. 5). The quartz boat was equipped with a chromel - alumel thermocouple (diameter 0.3 mm), placed in a powder. The thermocouple was not touching the walls of the boat. In a number of experiments, after synthesis and cooling to room temperature, the reactor was placed in an external bath of a HAAKE-Q cryostat (Germany), cooled to 0–35 °C in an argon flow using ethyl alcohol as a refrigerant [34]. After reaching the required temperature, the argon flow was replaced with a dry air flow to passivate the nanopowder. For drying, air was passed through a column with solid alkali (KOH) 0.6 m long and turns of a flexible hose placed in the inner bath of the cryostat. The heating of the powder after replacing the gas streams indicated the beginning of the process of interaction with air. Fig. 5. Diagram of the experimental setup, 1 - HAAKE-Q cryostat, 2 - external cooling bath, 3 - thermal insulation, 4 - loop of a flexible hose for air drying, 5 - ethyl alcohol, 6 - hole for filming. If ignition occurred, the sample surface changed color from black to yellow-green (WO3 yellow-green). If there was no ignition within 30 minutes, the air flow was replaced with an argon flow and the reactor was heated to room temperature. Then the quartz boat with the passivated powder was removed from the reactor and immediately placed on a nickel foil to avoid ignition. Then, a nickel foil with nanopowder was placed on a stage for video recording. The process of removing the boat and placing the nanopowder on the table took about 5 s. In another series of experiments, the W nanopowder was passivated at 20 °C for 1 hour in an argon flow containing 3% air. To establish the combustion modes of W nanopowders, a Nikon 1 color video camera (30 frames per second) and a Flir 60 infrared camera (30 frames per second, 320x240 pix, sensitivity interval 8 - 14 m) were used. The phase composition of the obtained samples was studied using a DRON 3M X-ray diffractometer (Russia) with a coordinate-sensitive detector. The specific surface area was measured using a Sorbi-M analyzer by the BET method. Nanopowders obtained by chemical metallurgy at 480 °C from all three starting WO3 powders used are pyrophoric. Typical sequences of video frames of self-ignition and combustion in air of a synthesized nanopowder from (WO3 (1), 2-mm layer thickness) are shown in Fig. 6a. A sequence of IR video frames of a nanopowder burning in air (initial WO3 powder (1), 2 mm thick) obtained under the same conditions is showed in fig. 6b. As seen from Fig. 6, the combustion front appears at the edge of the samples and spreads to the center of the backfill. The maximum combustion temperature exceeds 670 °C. Powders obtained from samples WO3 (2) and WO3 (3) burn in the same way. Nanopowders -W obtained at 640 °C from all used initial WO3 powders are not pyrophoric, because at a temperature of 20 °C in air, they do not ignite spontaneously. Self-heating of samples taken from the reactor immediately after synthesis does not lead to the propagation of the flame front. However, after the completion of the stage of self-heating and cooling of the samples to room temperature, the combustion of any sample of W nanopowder can be initiated with a heated wire. Upon initiation by a heated wire, the combustion mode of the -W nanopowder, as can be seen from Fig. 7a is finger-like. A sequence of frames of infrared video recording of self-heating in air for samples of -W nanopowder (initial temperature 20 °C) of various thickness (1.2.3 mm, from left to right) obtained by the method of chemical metallurgy at 640 °C is shown in Fig. 7b (2 left frames). Fig. 6. a) Combustion in air of a nanopowder obtained by chemical metallurgy at 480 °C (sample 1, 2 mm thick); 20 °C, 30 frames per second. The time in seconds on each frame bottom right after the video mode was turned on. b) A sequence of frames of infrared video recording of a nanopowder burning in air (sample 1, 2 mm thick) obtained by the method of chemical metallurgy at 480 °C, initial temperature 20°C, 30 frames per second. On each frame bottom right, the time (minutes-seconds) after the video mode was turned on. Self-heating of samples removed from the reactor immediately after synthesis (Fig. 7b, 2 left frames) does not lead to the propagation of the flame front. However, after the completion of the stage of self-heating and cooling of the samples to room temperature, combustion of any sample of nanopowder W can be initiated with a heated wire (two right frames in Fig.7b). As seen from Fig. 7b, the initiated sample burns nonuniformly, the maximum temperature of the sample at the “tip” of the “finger” exceeds 670 °C. Fig. 7. a) Initiated combustion in air of W nanopowder (initial powder of grade (1)) obtained by chemical metallurgy at 640 °C (sample 2 mm thick). Initial temperature 20 °C. On each frame bottom right, the time in seconds after initiation. b) A sequence of frames of infrared video recording of self-heating in air for samples of -W (initial temperature 20 °C) of various thickness (1.2.3 mm, from left to right) obtained by the method of chemical metallurgy at 640 °C (two left frames). The two right frames show the initiated combustion of the central sample, 2 mm thick. On each frame bottom right the time (minutes - seconds) after turning on the video recording mode, The time dependences of heating W nanopowder obtained at 480 °C from grade 1 tungsten oxide on time during passivation in a dry air flow at initial temperatures of –34 °C (squares), –30°C (bold circles), and –24 °C (circles) are shown in Fig. 8. Zero time corresponds to the moment of replacing the argon flow with a passivating dry air flow. As can be seen from the figure, the maximum heating at the initial passivation temperature - 24 °C is 170 °C. In this case the color of the sample changes to yellow. Heating at -30 °C is ~ 20 °C, heating at -35 °C is ~ 0 °C. In both cases, the samples do not change color. The relatively small values of heating at T0 = - 30 °C are probably associated with the release of heat during the passivation of tungsten nanoparticles. However, unlike iron and nickel nanopowders, this method of processing the obtained nanopowders did not provide passivation of the W nanopowder, since the sample ignites spontaneously on contact with air. The ignition of the nanopowder was avoided if it was placed on a nickel foil immediately after being removed from the reactor. Thus, passivation at temperatures below zero proved to be ineffective without additional heat removal into the metal foil. Therefore, in the main series of experiments, passivation was carried out at room temperature for 1 hour in an argon flow containing 3% air. This procedure excluded self-ignition of the nanopowder upon contact with air. For all three precursors used, the specific surface areas of nanopowders, determined by the BET method, both for those obtained at 480 °C (passivated) and at 640 °C (not passivated), were 15 ± 3 m2/g and 9 ± 3 m2/g, respectively. For all three precursors used, X-ray phase analysis of W nanopowders obtained at 640 °C showed that they contain only -W (Fig.9a). Passivated nanopowders obtained at 500 °C from tungsten oxide grades 1 and 2 contain -W, -W and WO2.9 (рис.9б). Fig. 8. Time dependence of sample heating during passivation at - 34 °C (squares), - 30 °C (bold circles) - 24 °C (circles). Zero time corresponds to the moment of replacing the argon flow with a dry air flow. A sample of W nanopowder obtained from grade 3 tungsten oxide at 480 °C contains only -W and traces of WO2.9 and WO3 (Fig.9d), the presence of which is obviously associated with the passivation procedure. It should be noted that the temperature range of W, synthesis obtained in this work is very narrow: 470 ÷ 490 °C, while in [24] the optimal temperature was 500 °C. For comparison, the XRD analysis of a nanopowder obtained from grade 2 tungsten oxide at 480 °C is showed in fig. 9c. It can be seen that this nanopowder is a mixture of -W, -W, WO3 and WO2.9. Above 640 °C, only W is obtained. Here are the main results of this section. Tungsten nanopowders are synthesized by reduction of tungsten trioxide with hydrogen (chemical metallurgy method) at 440 ÷ 640 °C from samples with different specific surface: 2 m2/g (1), 11 m2/g (2), 0.8 m2/g (3). It is shown that the W nanopowder synthesized at 640 °C for all three precursors used is non-pyrophoric. Its combustion can be initiated by an external source. Combustion develops in a spatially non-uniform regime. Nanopowder synthesized at 480 °C from tungsten oxide grades 1 and 2 is a mixture of -W, -W and WO2.9; this powder is pyrophoric. It was found that the passivated W nanopowder synthesized at 480 °C from grade 3 tungsten oxide is W with traces of WO3 and WO2.9. Temperature range of synthesis W, obtained in the work is very narrow: 470÷490 0C. Fig. 9.a) X-ray phase analysis of W nanopowder obtained at 640 °C and passivated in an argon flow containing 3% air at a temperature of 20 °C (starting powder of grade (1)). b) X-ray phase analysis of nanopowder obtained at 500 °C and passivated in an argon flow containing 3% air at a temperature of 20 °C (original powder of grade (2)). c) X-ray phase analysis of a nanopowder obtained at 480 °C and passivated in an argon flow containing 3% air at a temperature of 20 °C (original powder of grade (2)). d) X-ray phase analysis of W nanopowder obtained at 480 °C and passivated in an argon flow containing 3% air at a temperature of 20 °C (original powder of grade (3)). The specific surface area of -W nanopowders is 10 ± 2 m2/g; for the -W mixture with traces of WO3 and WO2.9 it is 18 ± 1 m2/g. The dynamics of temperature fields during the ignition and combustion of tungsten nanopowders obtained at different temperatures has been studied. §3. Combustion of compacted samples of iron nanopowders. Literature data on the preparation and properties of compact samples from nanopowders are rather limited. In [35], the features of flame propagation over tablets made from mixtures of Al/CuO nanopowders (so-called nanothermites) were studied as a function of the density during laser initiation of combustion. It was found that less dense samples (porosity 90%) ignite faster and the speed of flame propagation in them is an order of magnitude higher than in denser samples (porosity 50%). According to the authors, these results indicate a change in the combustion mechanism with an increase in the density of the compacted sample from convective to diffusion. Similar measurements described in monograph [36] were carried out with samples of Al/MoO3 nanopowders, and the results obtained for this nanothermite are qualitatively the same. It should be noted that there are no data in the literature on the regularities of spontaneous ignition and self-heating of compacted samples. This section describes the experimental establishment of the combustion features of compact samples of non-passivated iron nanopowders and the effect of the porosity of these compact samples on the dynamics of their heating in air. Experimental part In this work, for experimental studies of the processes of ignition and passivation, iron nanopowders obtained by the chemical-metallurgical method were used. The main stages in the synthesis of metal nanopowder are the deposition of metal hydroxide, drying, and reduction [37]. The synthesis of iron hydroxide was carried out by heterophase interaction of a solid metal salt with an alkali solution. After precipitation of iron hydroxide, it was first washed in a Buchner funnel to pH = 7 and then dried in air until dusting. To obtain a metal nanopowder, iron hydroxide powder was reduced in a furnace for 1 h at 400 °C in a hydrogen flow in a reactor (the reactor is schematically shown in Fig. 5). Then the reactor was removed from the furnace and cooled in air to 20 °C in an argon flow. Then a quartz boat 19 cm long and 3 cm wide with nanopowder was transferred from the reactor to a portable quartz vessel filled with argon at atmospheric pressure. In a separate series of experiments, a quartz boat with nanopowder was removed from the reactor and placed on a stage for filming using a Flir 60 infrared camera (60 frames/s, 320x240 pix, sensitivity interval 8–14 m). The compaction of nanopowders was carried out in an original installation equipped with a heated mould (Fig. 10). The installation includes a sealed box with scales, a press, a gateway, and electrical inputs for connecting heating, initiation and measurement devices, as well as a heated mould, into which the required amount of non-passivated iron nanopowder was placed. The installation makes it possible to obtain compact products even from pyrophoric (non-passivated) nanopowders, because all operations with nanopowders, from opening vessels with nanopowders, weighing and pressing them to heating the samples, are carried out in a sealed box filled with an inert gas (argon) and equipped with a gateway for changing powders and samples. Cylindrical compact samples with a diameter of 5 mm, a length of 7.7–11.8 mm, and a density of 2.55–3.84 g/cm3 were obtained from iron nanopowder [37] and also studied. Fig. 10. General view of the installation (a sealed box with scales, a press, a sluice and electrical inputs for connecting heating, initiation, measuring devices) and a mould. The peculiarity of the mould is the possibility of programmed heating of samples pressed from metal powders in an inert gas atmosphere. To control the heating temperature in the lower punch of the mold (1) there is a slot for installing a U-shaped thermocouple 50-100 μm thick (2), isolated from the punch (1), the mould (3) and the upper punch (4). To reduce heat loss, the powder being pressed is separated from the punches by heat-insulating gaskets. The signal from the thermocouple is recorded to a computer through an analog-to-digital converter with a frequency of 1 kHz. A Flir 60 infrared camera and a SONY - FDR - AX - 33 video camera were used to study the change in the temperature distribution over the sample surface over time and to determine the maximum temperature at each time point. The temperature of the upper end of the sample was recorded with an infrared camera. Results and discussion The typical results of optical filming of the combustion of cylindrical samples made of iron nanopowder a) 7.7 mm high and 3.84 g/cm3 and b) 9.5 mm high and 3.22 g/cm3. It should be noted that self-ignition of the sample (there is no external initiation) begins from the top end, which is least screened from the oxidizer, and, as will be shown below. Self-ignition occurs almost immediately on the entire end surface. As seen from Fig. 11, a combustion wave propagates downward from the upper end of the sample at an approximately constant velocity. Fig. 11. Results of optical filming of the combustion of cylindrical samples made of iron nanopowder a) in height of 7.7 mm and a density of 3.84 g/cm3 b) in height of 9.5 mm and density of 3.22 g/cm3. Estimations of the combustion rate V, determined from three points on the combustion front, which is visualized very clearly in the form of a horizontal dark stripe, give for the sample a) V ≈ 0019 cm/s, and for the sample b) V ≈ 0047 cm/s. This means that the rate of flame propagation in a less dense sample a) is noticeably higher than in a denser sample b), that is, the process of transfer of the oxidant into the sample plays an important role in the combustion of compacted samples of iron nanopowders. This result is similar to the results obtained in [35, 36] for the initiated combustion of nanothermites. Let us consider the change in the combustion temperatures of samples of different density during self-ignition. Typical frames of self-ignition and combustion of samples of iron nanopowder 1 mm thick (on the left in each frame) and 4 mm (on the right in each frame) immediately after extraction from the reactor into atmospheric air are shown in fig. 12. It can be seen that a thinner sample heats up more weakly due to a more intense heat dissipation. A red triangle indicating the maximum temperature is located on a sample 4 mm thick in all frames. Fig. 12. Typical frames of self-ignition and combustion of samples of iron nanopowder 1 mm thick (on the left in each frame) and 4 mm (on the right in each frame) immediately after being removed from the reactor. It can be seen from fig. 12 that the maximum combustion temperature of the bulk iron nanopowder sample is 560 °C (5th frame at 26 s). With an increase in the density of compacted samples, the maximum combustion temperature decreases. For example, typical frames of the combustion of a compacted sample of iron nanopowder with a density of 2.91 g/cm3 are shown in fig. 13. Fig. 13. Typical frames of combustion of a compacted sample of iron nanopowder with a density of 2.91 g/cm3. The first two frames (top left) show the transfer of the sample from the compaction unit to the stage for filming. It can be seen (5th frame at 1 min 6 s) that the maximum combustion temperature of the compacted sample is less than the maximum temperature reached during the combustion of the backfill (see Fig. 12). With an increase in the compact density, the maximum combustion temperature decreases. This is illustrated in Fig. 14, which shows the dependences of the maximum combustion temperature on time for compacted samples of different densities. Fig. 14. Dependences of the maximum combustion temperature on time for compacted samples of different densities: a) 2.91 g/cm3, b) 3.37 g/cm3, c) 3.84 g/cm3. The results obtained mean that the propagation velocity of the combustion front and the maximum combustion temperature of compacted samples made of non-passivated iron nanopowders decrease with increasing compact density. Since earlier similar regularities were observed for the initiated combustion of nanothermites (Al + CuO, Al + MoO3) [35, 36], it can be assumed that these regularities are general for combustible or pyrophoric nanosystems. Conclusions for Chapter 8 Copper nanopowders are obtained by the method of hydrogen reduction (chemical-metallurgical method) and thermal decomposition of copper citrate and formate. It was shown that copper nanopowder synthesized from copper citrate is not pyrophoric. Combustion of this copper nanopowder can be initiated by an external source, with the combustion wave velocity being 1.3 ± 0.3 mm/s. The nanopowder has a ~ 4 times larger specific surface area than the nanopowder obtained by the chemical-metallurgical method. It practically does not contain oxides and is stable in atmospheric air. Copper nanopowder obtained by the chemical-metallurgical method is pyrophoric and therefore requires passivation, but its passivation leads to the formation of noticeable amounts of copper oxides. The burning rates of passivated and non-passivated copper nanopowder obtained by the chemical-metallurgical method are the same. Tungsten nanopowders are synthesized by reduction of tungsten trioxide with hydrogen (chemical metallurgy method) at 440 ÷ 640 °C from samples with different specific surface. It is shown that the W nanopowder synthesized at 640 °C for all three precursors used is non-pyrophoric -W. Its combustion can be initiated by an external source. Combustion continues in a spatially non-uniform regime. Nanopowder synthesized at 480 °C from tungsten oxide grades 1 and 2 is a mixture of -W, -W and WO2.9. This powder is pyrophoric. It was found that the passivated W nanopowder synthesized at 480 °C from grade 3 tungsten oxide is W with traces of WO3 and WO2.9. Temperature range of synthesis W, obtained in the work is very narrow: 470÷490 0C. The specific surface area of -W nanopowders is 10 ± 2 m2/g; for the -W mixture with traces of WO3 and WO2.9, it is 18 ± 1 m2/g. The dynamics of temperature fields during the ignition and combustion of tungsten nanopowders obtained at different temperatures has been studied. Preliminary experimental studies of the combustion features of compact samples made of non-passivated iron nanopowders and the effect of the porosity of these compact samples on the dynamics of their heating in air have been carried out. The aim is to determine the temperature range at which it is possible to carry out safely technological operations with compact samples of non-passivated iron nanopowders. It was found that the propagation velocity of the combustion front and the maximum combustion temperature of compacted samples made of non-passivated iron nanopowders decrease with increasing compact density.

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