In the early 1970's a new processing technique to produce metallic alloys was developed by Benjamin and co-workers. This novel technique, called Mechanical Alloying (MA), involves the repeated welding, working hardening, and fracture of metallic powders to form an alloy. The research presented in this thesis describes the use of the MA process to form polymer blends. Until recently there has been no published work discussing the possibility of using this technique with polymers. This research lays the ground work for using the MA process to produce polymer blends by comparing this technique to conventional polymer processing techniques. The MA process was used to form blends of polypropylene (PP) and a liquid crystalline polymer (LCP). Samples were prepared and then characterized using thermal analysis via differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Mechanical testing, Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD) were performed on the materials. Scanning electron micrographs (SEM) of fracture surfaces are also presented. The results suggest that the solid state mechanical alloying process is a viable technique to form polymer blends. / Master of Science

Titanium been used industrially for nearly a century. Ever since it was first reduced to its elemental form, concerted efforts have been made to improve the material and to reduce the cost of production. In this thesis, titanium is mechanically alloyed with cellulose nanocrystals followed by powder consolidation and sintering to form a solid titanium metal matrix composite. Cellulose nanocrystals (CNCs) were chosen as the particle reinforcement as they are a widely abundant and natural material. Additionally, the nanocrystals can be derived from waste materials such as pistachio shells. This offers a unique advantage to act as a green process to enhance the mechanical properties of the titanium as well as to reduce to cost of production. Vibrational milling using a SPEX 8000M mill was used to mechanically alloy titanium powder with varying concentrations of CNCs. Additionally, the milling time was varied. This process showed that varying the concentrations of CNCs between 0.5% - 2% by weight did not noticeably alter the microstructural or mechanical properties of the materials. Conversely, changing the milling time from 0.5 hours to 5 hours proved to greatly alter the microstructural and mechanical properties of the titanium matrix metal composites. Further increasing the milling time to 10 and 25 hours caused the materials to become exceedingly brittle thus, the majority of experiments focused on samples milled between 0.5 hours and 5 hours. The hardness values for the Ti-1%CNC materials increased from 325-450-600-800 for the samples milled for 0.5, 1, 2, and 5 hours respectively. The other concentrations used were found to yield similar values and trends. SEM micrographs showed that small precipitates had formed within the grains except materials milled at 5 hours, which showed the production of very coarse particles at the grain boundaries. Similarly, an attrition mill was used to mechanically alloy titanium with varying CNC concentrations. Milling time was also varied. The powders were consolidated, sintered and characterized. It was found that increasing CNC content at low milling times caused a reduction in hardness. The X-ray diffractograms also showed a trend in that the diffraction patterns shifted to the lower angle with increasing CNC concentration, thereby suggesting that the increase in CNC content facilitated the removal of oxygen atoms housed within the interstitial sites. The oxygen was observed to diffuse and precipitate platelet titanium dioxide particles. These particles were found to be located within the titanium grains and coarsened with milling time. Generally, increasing the milling time to 15 hours was found precipitate particles at the grain boundaries as well as to excessively dissolve oxygen into the titanium lattice leading to embrittlement. The materials milled for 5 hours showed the best increase in strength while maintaining good ductility. / Master of Science / Titanium has only been used industrially since the early 1940’s thanks in large to the modern advances to reduce titanium ore to its elemental state. Titanium gained much interest as a structural material because of its corrosion resistance and its exceptional strength for a lightweight metal, making the material ideal for medical and aerospace applications. Pure titanium was found to be soft and had poor wear resistance, therefore, efforts were made to create titanium alloys which mitigated these weaknesses. Often titanium is alloyed with costly and toxic elements to enhance its strength properties, making it dangerous to use in the medical field. One way to enhance the strength properties of titanium without the addition of these harmful alloying elements is to create a titanium composite by adding strong inert particles to a titanium matrix. One method to create titanium metal matrix composites is to violently mix titanium powder with the reinforcement material, through a process called mechanically alloying. Following the mixing process the powder is then compacted and heated to form a solid part through a process called sintering. While these powder processing methods are known and viable for forming titanium metal matrix composites, some of the reinforcement materials can be expensive. In this thesis, cellulose nanocrystals (CNCs) will be added as reinforcement to titanium by means of two mechanical alloying processes, vibratory milling (shaking) and attrition milling (stirring). CNCs can be derived from plant matter which is widely abundant and inexpensive. The viability of CNCs to be used as a reinforcement material, as well as the mechanical alloying processes were investigated to determine the effect on the titanium strength properties. The powder processing steps were found to cause the CNCs to react with the surrounding titanium matrix which caused beneficial oxides to form as the reinforcement materials. In general, it was found that vibratory milling caused the final titanium metal matrix composite to be hard and brittle. Attrition milling was found to be more favorable as some materials were observed to be strong yet ductile.

Metal Matrix Composites (MMCs) are used as structural materials because of their ability to have a combination of high strength and good ductility. A common problem with MMCs utiliz-ing vastly different materials is the difficulty in forming a strong matrix/reinforcement interface without suffering extensive dissolution, debonding, or chemical reactions between the compo-nents. In this work, a nickel base amorphous particulate reinforced crystalline nickel matrix composite is processed. The reinforcement, an equimolar NiW amorphous powder, was synthe-sized using the mechanical alloying process. The amorphous and crystalline nickel powders were blended in varying volume fractions and then consolidated using hot-isostatic pressing (HIP). This work reveals that the amorphous NiW reinforcement provides strength and hardness to the ductile Ni matrix while simultaneously maintaining a strong interfacial bond due to the similar chemistry of the two components. The strengthening achieved in the composite is attrib-uted to the particulate/matrix boundary strengthening. / Master of Science

Mechanical alloying, compaction by cold isostatic pressing, and pressureless sintering were used to study the potential for W â 3 wt% Ni â 1 wt% Fe to be processed into the bulk nanocrystalline form as a replacement material for depleted uranium in kinetic energy penetrators. Milling time and sintering temperature were varied from 15 to 100 hours and 1000 to 1300°C respectively. Particle size analysis and SEM showed a bimodal particle size distribution with most of the particles below 10 µm in size. XRD peak broadening analysis showed crystallite size to be reduced to below 50 nm, while peak shifting indicated a reduction in W lattice parameter due to dissolution of Ni and Fe atoms into the W BCC lattice. Post-sintering bulk characterization showed density increasing strongly with increasing sintering temperature to above 90% of theoretical density at 1200°C. Apparent activation energy for sintering decreased strongly with increasing milling time. SEM micrographs showed a bimodal grain size distribution with some areas of smaller submicron grains and others with larger grains on the order of 1 – 4 µm, likely connected to the bimodal particle size distribution from milling. XRD and SEM also showed the precipitation of two secondary phases during sintering: (Fe, Ni)6W6C incorporating carbon from the grinding media and an FCC solid solution of Ni, Fe, and W. The intermetallic carbide phase will increase strength but reduce ductility of the bulk material, which is not desirable. Micro and macrohardness testing show similar trends as density with a strong correlation with sintering temperature. / Master of Science

Reinforcing metals with compositionally similar amorphous particles has been found to create composites with good interfacial bonding. It is conceivable that significant additional strengthening in amorphous reinforced composites can be realized by creating high-aspect ratio reinforcements; attritor milling holds promise in this regard. In this work, mechanical alloying was used to produce equimolar Ni-W powder that became a composite of amorphous Ni-W with undissolved W crystallites. A mixture of nickel powder and ten volume percent amorphous Ni-W powder was blended by attritor milling for either one or three hours, compacted by combustion-driven compaction and sintered for up to fifty hours at 600ºC. Prolonged times at elevated temperatures led to crystallization of the amorphous reinforcement particles and dissolution of tungsten into the matrix. Vickers macrohardness tests on the sintered composites yielded lower-than-expected values. Microscopy after hardness testing revealed sliding of particles at their boundaries, indicating poor bonding between them. It is believed that the sintering process was compromised by contamination from organic vapor present in the tube furnace used. While attritor milling effected smaller reinforcement particles, the small increase in aspect ratio would likely have been insufficient to cause significant strengthening by shear load transfer. / Master of Science

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Submitted by Kamila Costa (kamilavasconceloscosta@gmail.com) on 2015-08-06T14:48:56Z No. of bitstreams: 1 Dissertação - Zeane V Borges.pdf: 2189307 bytes, checksum: 3fce099edb43ceed11ff4ab744e1f3f5 (MD5) / Approved for entry into archive by Divisão de Documentação/BC Biblioteca Central (ddbc@ufam.edu.br) on 2015-08-07T14:07:07Z (GMT) No. of bitstreams: 1 Dissertação - Zeane V Borges.pdf: 2189307 bytes, checksum: 3fce099edb43ceed11ff4ab744e1f3f5 (MD5) / Approved for entry into archive by Divisão de Documentação/BC Biblioteca Central (ddbc@ufam.edu.br) on 2015-08-07T14:08:30Z (GMT) No. of bitstreams: 1 Dissertação - Zeane V Borges.pdf: 2189307 bytes, checksum: 3fce099edb43ceed11ff4ab744e1f3f5 (MD5) / Made available in DSpace on 2015-08-07T14:08:30Z (GMT). No. of bitstreams: 1 Dissertação - Zeane V Borges.pdf: 2189307 bytes, checksum: 3fce099edb43ceed11ff4ab744e1f3f5 (MD5) Previous issue date: 2015-06-08 / FAPEAM - Fundação de Amparo à Pesquisa do Estado do Amazonas / The nanostructured SnSe2 alloy was produced by Mechanical Alloying technique and their structural, thermal and optical properties were investigated by x-ray diffraction (XRD) combined with Rietveld Method (RM), differential scanning calorimetry (DSC), absorbance measurements and photoacoustic absorption spectroscopy (PAS). After characterized in the as milled conditions, the sample was annealed at 450˚C in order to evaluate the influence of the interfacial component in their physical properties. The XRD measurements allowed structurally characterize the samples, as well quantify the volume fractions occupied by crystalline and interfacial components. The DSC measurements showed that the melting process of SnSe2 phase, occurs in two-step for both samples. The UV–Vis absorption spectrum showed direct allowed transitions for milled and annealed samples, with band gap of 1.02 eV and 1.48 eV, respectively. Moreover, electronic transition of type direct forbidden was found in the sample annealed with optical band gap of 0.94 eV. PAS measurements provided the thermal diffusivity (𝛼𝑠) for both samples. A reduction of 45% in the thermal diffusivity value of milled sample was observed, when compared with the annealed sample. / A liga nanoestruturada SnSe2 foi produzida pela técnica Mechanical Alloying e suas propriedades estruturais, térmicas e ópticas foram investigadas por difração de Raios X (DRX) combinado com o Método de Rietveld (MR), calorimetria diferencial de varredura (DSC), medidas de absorbância óptica e espectroscopia de absorção fotoacústica (PAS). Após caracterizada nas condições como moída, a amostra foi tratada termicamente na temperatura de 450˚C a fim de avaliar, a influência da componente interfacial nas suas propriedades físicas. As medidas de DRX permitiram caracterizar estruturalmente as amostras, bem como quantificar as frações volumétricas ocupadas pelas componentes cristalina e interfacial. Medidas de DSC mostraram que o processo de fusão da fase SnSe2, ocorre em duas etapas para ambas as amostras. Os espectros de absorção UV-Vis mostraram transições diretas permitidas para as amostras moída e tratada termicamente, com energias de band gap de 1.02 eV e 1.48 eV, respectivamente. Além disso, transição eletrônica do tipo proibida direta foi encontrada na amostra tratada com energia de band gap de 0.94 eV. Medidas de PAS forneceram o valor da difusividade térmica (𝛼) para ambas as amostras. Uma redução de aproximadamente 45% no valor da difusividade térmica da amostra moída, quando comparada com a amostra tratada termicamente, foi observada.

A thesis submitted to the Faculty of Engineering and the Built Environment, University of the Witwatersrand, in fulfillment of the requirements for the degree of Doctor of Philosophy, Johannesburg, August 2017 / Titanium aluminides Ti3Al (α2), γ-TiAl and TiAl3 have received much attention for potential applications where light weight for energy saving, room temperature corrosion resistance in aqueous solutions, high-temperature oxidation resistance, or where combinations of the above are needed. Gamma-TiAl of composition Ti-47.5 at.% Al with additions of platinum group metals (PGMs: Pt, Pd, Ru and Ir) was investigated for microstructure, hardness, room temperature aqueous corrosion, high-temperature oxidation resistance, mechanical alloying and consolidation by spark plasma sintering, and coating on titanium Grade 2 and Ti-6Al-4V substrates. Gamma-TiAl of Ti-47.5 at.% Al produced by melting and casting gave a microstructure consisting of γ grains and lamellar grains with alternating of α2 and γ phase lamellae. Additions of 0.2, 1.0, 1.5, and 2.0 at.% PGMs introduced new phases of high PGM contents. The γ and lamellar phases were still present. The additions of PGMs significantly improved the aqueous corrosion properties at room temperature, by improving the pitting corrosion resistance of the γ-TiAl alloy by modifying its hydrogen evolution of the cathodic reaction. The presence of PGMs also influenced the oxidation behaviour of γ-TiAl at 950°by forming the Z-phase which stabilized a continuous protective Al2O3 phase. However, Ti-47.5 at.% Al, being a two-phase alloy (α2+γ), PGMs could not sustain a stable Z-phase, as it transformed into an oxygen supersaturated Ti3Al, which subsequently led to the formation of TiO2+Al2O3, a non-protective oxide mixture. The optimal PGM addition to γ-TiAl was 0.5 at.%, with iridium giving the best room temperature corrosion and high-temperature oxidation resistance. Mechanical alloying of Ti and Al pure powders with PGM additions gave powders where α2 and γ were only identified after heat treatment. Consolidation of the mechanically alloyed powders by spark plasma sintering gave different microstructures from the cast alloys, with continuous α2 and γ phases and evenly distributed nanometer-sized alumina, and much higher hardnesses. Cold spraying the mechanically alloyed powders on to titanium Grade 2 and Ti-6Al-4V substrates gave coatings of irregular thickness, dense near the substrates with porosity at the top, giving poor oxidation protection. / CK2018

Neste trabalho, investigou-se a elaboração mecânica do composto intermetálico TiFe por moagem de bolas com alta energia. Uma forte aderência do material moído, particularmente nas paredes do recipiente de moagem, foi o principal problema verificado com tempos de moagem superiores a 1 hora (moinho agitador). Tentativas para resolver este problema foram realizadas inicialmente com o emprego de agentes controladores de processo (ACPs), como etanol, ácido esteárico, polietileno de baixa densidade, benzeno e ciclohexano, em diferentes quantidades (1 a 20% em massa) e tempos (1 a 40 h), mantendo-se constantes outros parâmetros de moagem como a razão bola:pó em massa (10:1) e o tamanho das bolas (=7mm). Os rendimentos mais elevados (em termos da massa de pó não aderido) foram obtidos quando se utilizaram grandes quantidades de benzeno e ciclohexano (101 e 103% em massa, respectivamente), porém com a formação de TiC ao invés de TiFe em razão da decomposição do ACP e reação do carbono com as partículas de titânio. As moagens foram realizadas posteriormente sem o emprego de qualquer ACP e também utilizando um moinho planetário. Várias estratégias foram investigadas para se tentar mitigar a aderência incluindo-se: (a) moagem de uma pequena quantidade da mistura de pós de Ti e de Fe, revestindo as paredes do recipiente e as bolas de moagem, antes da moagem da carga principal, (b) moagem pausada com aberturas intermediarias do recipiente em atmosfera ambiente, (c) moagem pausada para rotação e inversão da posição do recipiente de moagem (apenas no moinho agitador), (d) moagem isolada dos pós de Ti e de Fe, antes da moagem da mistura, e (e) moagem do pó de Fe com o Ti hidretado. Os melhores resultados, em termos de diminuição da aderência combinada com a formação majoritária do composto TiFe durante a moagem, foram obtidos quando se adotou o procedimento de inversão/rotação, juntamente com o processo de revestimento preliminar do recipiente e das bolas de moagem (26% em massa). Rendimentos maiores foram obtidos com a utilização do TiH2 no moinho planetário, porém sem a formação majoritária do TiFe durante a moagem. / In this work an investigation on the mechanical alloying of the intermetallic compound TiFe by high-energy ball milling was conducted. Strong adherence of milled material, particularly at the vial walls, was seen to be the main problem at milling times higher than 1 hour (shaker mill), hindering the compound synthesis. Attempts to prevent this problem were accomplished first by adding different process control agents (PCAs), like ethanol, stearic acid, low density polyethylene, benzene and cyclohexane at variable quantities (1 to 20 wt. %) and times (1 to 40 h), keeping constant other milling parameters like ball to powder mass ratio (10:1) and balls size (=7mm). Highest yields (related to the non adhered powder) were attained with larger amounts of benzene and cyclohexane (101 and 103 wt. %, respectively), but with TiC formation during milling instead of TiFe due to the PCA decomposition and the reaction of the carbon with and titanium particles. Milling was conducted further without adding any PCA and also using a planetary ball mill. Several strategies were tried to avoid or minimize the adherence including: (a) milling of a small quantity of the Ti and Fe powder mixture, dirtying the vial walls and the balls surfaces before milling the main charge, (b) stepwise milling with intermediate openings of the vial in air, (c) stepwise milling with the rotation and the inversion of the vial position between the steps (only in the shaker mill), (d) milling Ti and Fe powders (apart from each other) before milling the mixture of them, and (e) milling Fe powder with Ti hydride powder. Best results concerning both yield and major TiFe formation during milling were verified with the rotation/inversion procedure combined with preliminar dirtying of the vial and balls (26 wt.% in the shaker mill). Higher yields could be attained by using TiH2 powder in the planetary mill, but with no major TiFe formation during milling.

Depuis les années 90, dans le contexte de la pénurie annoncée d'énergies fossiles et de modifications climatiques, un regain d'intérêt s'est fait sentir pour les énergies renouvelables et, parmi elles, pour la thermoélectricité. Cette dernière permettant la conversion directe entre énergies thermique et électrique devrait permettre la récupération de l'énergie perdue sous forme de chaleur, durant les processus industriels. Cependant, à l'heure actuelle, l'efficacité de la conversion thermoélectrique, évaluée à partir du facteur de mérite, ZT, n'est pas suffisante pour des applications à grande échelle. Cependant, pour évaluer l'impact potentiel de la thermoélectricité, il est nécessaire de prendre en compte d'autres critères que celui de l'efficacité relativement faible de la thermoélectricité, qui la cantonne dans des niches spécifiques, et tels que la faible toxicité des matières premières, leur abondance, leur faible coût et leur facilité de mise en œuvre. Diverses familles de matériaux répondent à ces critères parmi lesquelles les plus favorables sont les siliciures pour les matériaux inorganiques et les polymères conducteurs pour les composés organiques. Dans ce travail de thèse, nous nous sommes intéressés au disiliciure de chrome (CrSi2) et au polymère PEDOT:PSS.Parmi les siliciures, CrSi2 est un candidat prometteur mais sa grande conductivité thermique est un handicap par rapport aux matériaux conventionnels. Elle peut cependant être réduite par nanostructuration. Nous présentons une étude CrSi2 nanostructurés (10-15 nm) obtenus soit par four à arc suivie d'un broyage mécanique, soit par mécanosynthèse. Ces poudres sont chimiquement stables jusqu'à 1073 K. A plus hautes températures, des phases secondaires apparaissent, notamment CrSi. Grâce à la technique SPS, CrSi2 a pu être densifié jusqu'à 94% en maintenant une taille nanométrique (30-45 nm) ce qui a conduit à une réduction de la conductivité thermique d'un facteur 2 par rapport au composé CrSi2 massif. Malheureusement, le facteur de mérite ZT n'a pas été amélioré en raison de l'accroissement de la résistivité électrique.Guidés par des calculs DFT, nous avons explorés de nouvelles voies de dopage pour améliorer les propriétés thermoélectriques de CrSi2. Des alliages Cr1-xTixSi2, Cr1-xZrxSi2 et Cr1-xMoxSi2 ont ainsi été synthétisés et nous avons étudié leurs propriétés thermoélectriques. A Tamb, le dopage au Ti semblerait de ne pas significativement améliorier le facteur de puissance (PF) pour une porosité de 11% par rapport à nano-CrSi2. Par contre, pour 2% Zr, PF a été amélioré d'un facteur 1.7 pour une porosité de 30%. En plus, il semblerait que le PF de Cr0.98Zr0.02Si2 avec une porosité de 0% est amélioré d'un factuer 1.9 par rapport au CrSi2 massif. Néanmoins, à hautes températures il existe encore un potentiel d'amélioration pour le dopage au Ti. Bien qu'il soit métastable, l'alliage Cr1-xZrxSi2 a pu être obtenu jusqu'à 5% Zr. Une optimisation supplémentaire est encore nécessaire pour les alliages dopés au Ti et Zr. L'alliage Cr1-xMoxSi2 est le plus prometteur avec une amélioration significative du facteur de Mérite (ZTmax > 0.2) pour 10% et 20% de Mo entre 500 et 700 K. Ces valeurs sont supérieures à celle du massif bien que toujours du même ordre de grandeur que le meilleur ZT obtenu pour CrSi2.Enfin, nous avons élaboré des composites à base de CrSi2 associé à du Polypyrrole (PPy) ou du PEDOT:PSS. Aucune amélioration significative n'a été obtenue pour le composite PPy-CrSi2. Dans le cas du PEDOT:PSS, nous avons testé la fonctionnalisation de CrSi2 pour améliorer sa dispersion dans le polymère. Nous avons montré qu'un agent de fonctionnalisation avec un groupement phosphonique réagissant avec Cr est le plus efficace. Cette étape est très prometteuse car il s'agit de la première étude de ce type effectuée dans le cas de l'élaboration de composites à base de siliciures intermétalliques pour des applications thermoélectriques. / In the context of renewable energies, which is related to the shortage of fossil energies and climate change, thermoelectricity has regained interest in recent years (1990s). The concept of this technology is the direct conversion between thermal and electrical energies. This can contribute to a progress in the industrial sector. However, the efficiency of the thermoelectric materials, denoted ZT (figure of merit), is not sufficient for large scale applications. Nevertheless, thermoelectricity can be found in the niche market sector where other criteria are taken into account such as the abundance of the raw elements, their price and toxicity. Several families meet these criteria with the silicides as inorganics materials and conductive polymers as organics materials being the most favorable. The objective of this dissertation was to investigate the chromium disilicide (CrSi2) and PEDOT:PSS.Among the silicides, CrSi2 stands as a promising candidate for thermoelectric applications. However, its relatively high thermal conductivity compared to the conventional materials is considered as a drawback. Therefore, we were interested in nanostructuration in order to reduce this thermal conductivity. Nanostructured CrSi2 is synthesized by arc melting followed by mechanical milling or mechanical alloying with a grain size of 10-15 nm. These powders have a good chemical stability up to 1073 K. Above this temperature, secondary phases, such as CrSi, are formed. SPS processing permits to efficiently densify our pellets up to 94% while maintaining nanometric grain size (30-45 nm). This leads to a reduction of the thermal conductivity by a factor of 2 compared to bulk CrSi2. However, the Figure of merit (ZT) does not improve as the electrical resistivity increases.DFT calculations predict that some doping elements have potentiality to improve CrSi2 electronic structure. Therefore, Cr1-xTixSi2, Cr1-xZrxSi2 et Cr1-xMoxSi2 alloys are synthesized in order to enhance the thermoelectric properties of CrSi2. At RT, The power factor of Cr0.9Ti0.1Si2 seems not to be improved compared to nano-CrSi2 for a porosity of 11%. On the other hand, 2% Zr doping improved the power factor by 1.7 at RT for a porosity of 30%. It also seems that for 0% porosity, the power factor of Cr0.98Zr0.02Si2 is improved by a factor 1.9 compared to bulk CrSi2. Nevertheless, an improvement could be predicted at high temperatures for Cr0.9Ti0.1Si2. Although Cr1-xZrxSi2 alloy is metastable, we were able to synthesize it by mechanical alloying up to 5%. Further optimization is needed for improving the thermoelectric performances of Ti and Zr- doped CrSi2 . On the other hand, Cr1-xMoxSi2 alloys seem to be the most promising as an increase of the Figure of merit is observed with a ZTmax reaching values larger than 0.2 for Cr0.9Mo0.1Si2 and Cr0.8Mo0.2Si2 in the temperature range of 500-700 K. These values are higher compared to the bulk but still in the same order of magnitude as for the highest ZT value report for CrSi2.We then elaborated CrSi2 based composites with Polypyrrole (PPy) and PEDOT :PSS. No significant enhancement was observed for PPy-CrSi2 composites. In order to improve the dispersion of CrSi2 in the PEDOT :PSS, we have tested the functionnalization. Preliminary tests show that grafting agents with phosphonic acid group is the most efficient by reacting with Cr. This step is very promising as no study till date reported the functionnalization approach for the elaboration of silicides based composites, especially for thermoelectric applications.