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Cryochemistry of Metal Nanoparticles

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Cryochemistry of Metal Nanoparticles Journal of Nanoparticle Research 5: 529–537, 2003. © 2003 Kluwer Academic Publishers. Printed in the Netherlands. Cryochemistry of metal nanoparticles Gleb B. Sergeev Laboratory of Low Temperature Chemistry, Chemistry Department, Moscow State University, 119899, Moscow, Russia (Tel.: +7(095)939 5442; Fax: +7(095)939 0283; E-mail: [email protected]) Received 20 March 2003; accepted in revised form 23 May 2003 Key words: metal nanoparticles, low temperature, solid state, encapsulation, sensor materials, spectroscopy, explosive reactions Abstract The interaction of metal atoms, clusters and nanoparticles with different organic and inorganic substances were studied at low temperature (10–40 K). Combination of matrix isolation technique and preparative cryochemistry was applied for the investigation of activity and selectivity of metal particles of different size. Encapsulation of metal nanoparticles in polymers was studied. The metal–polymer films thus obtained exhibited satisfactory sensitivity to ammonia. Introduction isolation technique and preparative cryochemistry. The interaction of metal particles with different organic The last decade of the 20th century was marked by the and inorganic substances will be presented in the first increased attention of scientists in the fields of physics, part of this article. In the second part we will consider chemistry, material science, etc., devoted to nanoparti- the encapsulation of metal nanoparticles in polymer cles, their synthesis, properties and different reactions. films and thus obtaining the nanosystems, exhibited The reason for this lies in the fact that particles of sensor activity. nanometer size exhibit peculiar properties. At present time the most interesting subject is the connection of chemical properties of metallic particles Reactions in low temperature with their size. Small metal particles with sizes in range co-condensate films from 1 to 10 nm exhibit high and sometimes unusual chemical reactivity and show a strong variation in their General remarks activity depending on cluster size. These are size effects in nanochemistry. The most successful are the study The method of low temperature chemistry is based of such effects in gas phase reactions and chemisorp- on the condensation of reagent vapors on the cooled tion. Simultaneous application of jet methods, pulsed surface in special cryostats under conditions, which laser characterization and different mass-spectroscopic exclude interaction in the gas phase. The scheme techniques allow to define the activity of metal par- in Figure 1 illustrates the fundamental possibility of ticles with different number of atoms (Binns, 2001; using low temperature in order to obtain metal clus- Knickelbein, 1999). ters, mono- and polynuclear metal complexes and Low and superlow temperature may be also used ligand-stabilized nanoparticles. for distinguishing the activity of metal atoms and Chemical interactions in low temperature co- nanoparticles (Sergeev, 2001; Sergeev & Shabatina, condensates begin with metal atoms. During the 2002). This method is based on combination of matrix condensation and annealing of the samples the two 530 Figure 1. Scheme of chemical processes taking place in metal/ligand co-condensates at low temperatures. Metal and ligand interactions start from atoms and proceed as a number of parallel and sequential reactions lead to aggregation and metal nanoparticles’ formation and formation of organometallic compounds and complexes of different nuclearity. competing processes take place: the aggregation of The size of metal particles, which can be formed by metal species and their stabilization in the matrix. Addi- such technique and their reactivity are determined by tion of ligand into the systems may cause the formation the combination of different experimental conditions. of metal particles of different size and their stabilization The main experimentally controllable factors are the or reaction with ligand molecules. The aggregation of substrate temperature, metal/ligand ratio, reagent con- metals atoms and interaction with ligands occur prac- densation rate and the rate of sample annealing. It was tically without activation barrier. The high reactivity shown that the lower is the temperature of the substrate of small metal species is the main difficulty in estab- surface, the less are the interactions, controlled by the lishing the relation between the size of the particles diffusion and the more the possible is the formation and their chemical activity. There are also problems of high energetic and reactive species at low tem- in producing and isolating the compounds with def- peratures. Low temperature co-condensates belong to inite compositions. The reactions shown in Figure 1 non-equilibrium dynamic systems, which possess the are complex multifactor processes taking place under internal accumulated energy. The metal/ligand ratio highly non-equilibrium conditions and for a wide or strongly affects the size of metal particles, obtained narrow distribution of the reactive species on their via low temperature co-condensation. Increasing this chemical activity. This fact is reflected usually in the ratio usually leads to raising of the part of clus- kinetics of low temperature processes. ters and the more aggregated metal particles. The The general scheme of our cryochemical synthe- component condensation rate has a complex effect sis and reactions with metals, encapsulated in organic, on the properties of low temperature co-condensate inorganic or inert polymer matrices are presented in film. The lifetime of such highly active species, as Figure 2. The first step is the co-condensation of metal metal atoms, their dimers or trimers, during the co- and ligand vapors on surface at low or very low tem- condensation on cold surface is inversely proportional perature. Thus we produce solid co-condensate film. It to the condensation rate and depends on the nature is possible to observe the stabilization or reactions of of relaxation and diffusion processes in the system. metal species in such films using IR, UV-vis and ESR Intensity of particle beam determines the number spectroscopy and electrical measurements. During the of collisions of atoms and molecules with surface annealing to room temperature the dispersion of metal and each other. Together with chemical nature of nanoparticles or metal-containing polymer films are reagents all mentioned factors determine the path- formed. At last we produce nanosized metal-containing way of processes leading, or not, to a reaction. Pro- organosols or solid films and use these materials cesses, which occur during the real condensation, are to study various chemical transformations, catalytic more complicated than the given scheme (Sergeev, activity, gas sensor properties. 2003). 531 METAL (M) ORGANIC OR INORGANIC In evaporation source of COMPOUND low temperature In constant temperature bath or vacuum set-up evaporation source EVAPORATION AND CO-DEPOSITION OF VAPOURS ONTO THE SURFACE AT REACTIONS OF METAL LOW TEMPERATURE ATOMS AND CLUSTERS SOLID CO- ESR-SPECTROSCOPY IR-SPECTROSCOPY CONDENSATE FILM ELECTROPHYSICAL SLOW HEATING UP TO UV-Vis-SPECTROSCOPY PROPERTIES ROOM TEMPERATURE TEM - ANALYSIS DISPERSION OF METAL NANOPARTICLES IN LIQUID ORGANIC SOLVENT (MONOMER) OR SOLID METAL-CONTAINING POLYMER FILM SLOW POLYMERIZATION OF MONOMER UNDER ARGON EVAPORATION OF UNREACTED MONOMER VISCOUS METAL COLLOID THIN METAL – CONTAINING SOLUTION POLYMER FILM metal content up to a few percent depending on experimental conditions; the same particle size STORAGE AT ROOM TEMPERATURE NANOSIZE METAL- CHEMICAL REACTIVITY CONTAINING MATERIAL CATALYTIC ACTIVITY (ORGANOSOL OR SOLID METAL-POLYMER FILM) GAS SENSOR PROPERTIES Figure 2. Cryochemical synthesis of metal nanoparticles and their reactions with various ligands. Reactions of magnesium species In the case of carbon tetrachloride we have the competition of chemical reactions and formation of dif- In organic chemistry of poly-halogen compounds it is ferent chemical intermediates and products: Grignard known that at ambient temperature carbon tetrachlo- reagent (CCl3MgCl), tri-chloromethyl radical (CCl3), ride does not react with bulk magnesium. The situation dichlorocarbene (CCl2). The reaction mechanism was changes dramatically in Mg-CCl4 co-condensates on studied in detail (Zagorsky and Sergeev,1990). cold surface at temperature, close to the temperature Magnesium clusters of different nuclearity can be of liquid nitrogen (77 K). In film co-condensates we stabilized in low temperature matrices upon depo- have reactions, which are presented by the following sition at 77 K. The process of cluster formation is scheme: simply controlled by changing the reagent ratio. Mag- nesium atoms initiate radical reaction resulting in a number of recombination products. Magnesium atoms H2O CCl3MgCl CHCl3 aggregate in the systems with Mg : RX ratio in the range 1 : 100 and yield the Grignard reagent. The par- CCl C Cl Mg + CCl4 3 2 6 ticle size and the C–Hal bond energy are important. Recently, we have studied the interaction of magne- C Cl C Cl 2 2 2 4 sium species with halogen butanes and compared the 532 yields of octane (product of recombination) with C–Hal after clusters and possibly the reactivity changes in the bond energy (Ivashko, 2001). The results are corre- row Mg2 ≥ Mg3 > Mg4 ≥ Mg. lated with the C–Hal bond energy and our scheme of IR-spectroscopic study of this system have shown reaction. that the only stable products of the reaction are C2Cl4 New data
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