FR2591412A1 - Method for the production of powders and a sealed microwave plasma reactor - Google Patents
Method for the production of powders and a sealed microwave plasma reactor Download PDFInfo
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- FR2591412A1 FR2591412A1 FR8518240A FR8518240A FR2591412A1 FR 2591412 A1 FR2591412 A1 FR 2591412A1 FR 8518240 A FR8518240 A FR 8518240A FR 8518240 A FR8518240 A FR 8518240A FR 2591412 A1 FR2591412 A1 FR 2591412A1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/218—Yttrium oxides or hydroxides
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J12/00—Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor
- B01J12/002—Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor carried out in the plasma state
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/126—Microwaves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/28—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from gaseous metal compounds
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- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/20—Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state
- C01B13/22—Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state of halides or oxyhalides
- C01B13/28—Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state of halides or oxyhalides using a plasma or an electric discharge
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0643—Preparation from boron halides
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
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- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
- C01B21/0763—Preparation from titanium, zirconium or hafnium halides
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/029—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of monosilane
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- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/03—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of silicon halides or halosilanes or reduction thereof with hydrogen as the only reducing agent
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- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
- C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
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- C01B35/04—Metal borides
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- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/212—Scandium oxides or hydroxides
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- C01G23/07—Producing by vapour phase processes, e.g. halide oxidation
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- C01G55/004—Oxides; Hydroxides
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/46—Generating plasma using applied electromagnetic fields, e.g. high frequency or microwave energy
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0894—Processes carried out in the presence of a plasma
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Abstract
Description
DESCRLPTION
La présente invention est relative à un procédé de fabrication de poudre et à un réacteur étanche à plasma micro-onde pouvant servir à la mise en oeuvre de ce procédé.DESCRLPTION
The present invention relates to a powder manufacturing process and to a sealed microwave plasma reactor that can be used to carry out this process.
L'invention a pour but de fournir une technique permettant d'obtenir des poudres de haute qualité à fine granulométrie (inférieure à un micron). The invention aims to provide a technique for obtaining high quality powders fine particle size (less than one micron).
A cet effet, l'invention a pour objet un procédé de fabrication de poudre, caractérisé en ce qu'on envoie un gaz réactif à travers un jet de plasma micro-onde, notamnent annulaire, puis on refroidit les produits de la réaction à leur sortie du jet de plasma. For this purpose, the subject of the invention is a process for the manufacture of powder, characterized in that a reactive gas is sent through a jet of microwave plasma, in particular annular plasma, and then the reaction products are cooled to their temperature. output of the plasma jet.
L'invention a également pour objet un réacteur étanche à plasma micro-onde, caractérisé en ce qu'il comprend: une torche à plasma micro-onde adaptée pour être reliée à une source de gaz plasmagène et pour créer un jet de plasma micro-onde ; des moyens pour faire passer un produit réactif à travers le jet de plasma ; une enceinte réactionnelle pourvue de moyens de refroidissement et dans laquelle débouche la torche; et des moyens d'allumage de la torche traversant à joint étanche la paroi de l'enceinte. The subject of the invention is also a sealed microwave plasma reactor, characterized in that it comprises: a microwave plasma torch adapted to be connected to a source of plasma gas and to create a micro-plasma jet wave ; means for passing a reagent product through the plasma jet; a reaction chamber provided with cooling means and into which the torch opens; and ignition means of the torch passing through tight seal the wall of the enclosure.
Suivant des caractéristiques avantageuses
- l'enceinte comprend une cloche en matière isolante reliée à la partie aval de la torche, et une enveloppe métallique prolongeant la cloche et pourvue de passages de circulation d'un fluide de refroidissement ;;
- les moyens de refroidissement de 1 'enceinte canprennent des moyens d'injection de jets de gaz de refroidissement convergeant vers un point de l'axe de la torche situé près de l'extrémité aval de celle-ci
- le réacteur ccrnprend un allumeur par court-circuit monté à coulissement étanche dans la paroi de 1 'enoeinte en regard de l'extrémité aval de la torche
- 1 'enoeinte comprend des moyens pour injecter un gaz de confulement tangentiellement à sa paroi interne
- la torche est du type double flux et comporte un conduit annulaire adapté pour être relié à la source de gaz plasmagène et entourant un canal central adapté pour être relié à une source dudit produit réactif.Following advantageous characteristics
- The enclosure comprises a bell made of insulating material connected to the downstream portion of the torch, and a metal casing extending the bell and provided with circulation passages of a cooling fluid;
the cooling means of the chamber can take means for injecting jets of cooling gas converging towards a point on the axis of the torch located near the downstream end thereof
the reactor comprises a short-circuit igniter mounted to slide tightly in the wall of the enclosure opposite the downstream end of the torch;
The enoeinte comprises means for injecting a conflation gas tangentially to its internal wall;
the torch is of the double flux type and comprises an annular duct adapted to be connected to the plasma gas source and surrounding a central channel adapted to be connected to a source of said reactive product.
Quelques exemples de mise en oeuvre de l'invention vont maintenant être décrits en regard des dessins annexés, sur lesquels
- la figure 1 est une vue schématique, partiellement en coupe longitudinale, d'un réacteur conforme à 1' invention
- la figure 2 représente en coupe longitudinale, à plus grande échelle, la région II de la figure 1 ; et
- la figure 3 est une vue analogue de la région III de la figure 1.Some examples of implementation of the invention will now be described with reference to the accompanying drawings, in which:
FIG. 1 is a schematic view, partly in longitudinal section, of a reactor according to the invention;
- Figure 2 shows in longitudinal section, on a larger scale, the region II of Figure 1; and
FIG. 3 is a similar view of region III of FIG.
te réacteur représenté dans son ensemble à la figure 1, d'axe général X-X vertical, est essentiellement constitué d'une torche à plasma micro-onde double flux 1, d'une enceinte réactionnelle 2 et d'un dispositif de collection de poudre 3. Tous les éléments du réacteur sont reliés de façon étanche les uns aux autres pour en isoler ccmplètement 1 'espace intérieur de 1' atmosphère environnante. La torche 1 et 1 'enceinte 2 sont fixées à un bâti-support non représenté. the reactor shown as a whole in FIG. 1, of general vertical axis XX, essentially consists of a double flux microwave plasma torch 1, a reaction chamber 2 and a powder collection device 3 All elements of the reactor are sealed to each other to completely isolate the interior space of the surrounding atmosphere. The torch 1 and 1 'enclosure 2 are fixed to a not shown support frame.
La torche 1, que l'on voit mieux à la figure 2, c'prend un corps annulaire 4 relié à un guide d'onde 5 à section rectangulaire (non représenté sur la figure 2) par l'intesddiaire d'un orifice dans lequel est disposé un embout de couplage électrique 6. Ce corps est traversé coaxialement avec un large jeu par deux tubes concentriques 7 et 8 d'axe
X-X, dont un tube extérieur 7 métallique et un tube intérieur 8 qui peut être métallique ou en une matière électriquement isolante et résistante à la chaleur telle que du quartz. Au-dessus du corps 4, le tube 8 est relié à une source d'un gaz réactif (non représentée), et le tube 7, par l'intermédiaire d'un raccord lateral 9, à une source d'un gaz plasmagène (non représentée).L'espace annulaire délimité entre les deux tubes est ferS par une soudure au-dessus du raccord 9 et est ouvert vers le bas. A l'intérieur du corps 4, un té de jonction 10 enserre le tube 7, et sa harpe est reliée électriquement à l'embout 6. Un couvercle supérieur 11 ferme le corps 4 et entoure le tube 7 à joint étanche. Un manchon 12 pourvu d'orifices 13 d'admission d'un gaz de gainage est fixé autour de l'ouverture inférieure du corps 4 et entoure coaxialement les tubes 7 et 8 avec un large jeu. tes tranches d'extrémité inférieure des deux tubes 7 et 8 et du manchon 12 se trouvent à peu près dans le même plan horizontal.The torch 1, which is better seen in FIG. 2, comprises an annular body 4 connected to a rectangular section waveguide 5 (not shown in FIG. 2) through the interior of an orifice in FIG. which is arranged an electrical coupling tip 6. This body is coaxially traversed with a wide clearance by two concentric tubes 7 and 8 axis
XX, including an outer tube 7 metal and an inner tube 8 which may be metallic or an electrically insulating material and resistant to heat such as quartz. Above the body 4, the tube 8 is connected to a source of a reactive gas (not shown), and the tube 7, via a lateral connection 9, to a source of a plasmagenic gas ( not shown) .The annular space delimited between the two tubes is ferS by a weld above the connector 9 and is open downwards. Inside the body 4, a joining tee 10 surrounds the tube 7, and its harp is electrically connected to the tip 6. An upper lid 11 closes the body 4 and surrounds the tube 7 with a seal. A sleeve 12 provided with openings 13 for admitting a cladding gas is fixed around the lower opening of the body 4 and coaxially surrounds the tubes 7 and 8 with a wide clearance. The lower end slices of the two tubes 7 and 8 and the sleeve 12 are approximately in the same horizontal plane.
L'enceinte 2 est constituée d'une cloche en verre 14 équipée d'un dispositif d'allumage 15 et prolongée vers le bas par une enveloppe 16 en acier inoxydable. The chamber 2 consists of a glass bell 14 equipped with an ignition device 15 and extended downwards by a casing 16 of stainless steel.
La cloche 14 se termine vers le haut par un col 17 présentant un bourrelet d'extrémité 18. Ce col entoure la partie courante du manchon 12, et une paire de brides horizontales 19, 20, prenant appui sur le bourrelet 18, écrase un joint torique 21 entre la tranche d'extrémité du col 17 et la surface extérieure du manchon 12, au moyen de boulons non représentés, pour assurer l'étanchéité. The bell 14 ends upwards by a neck 17 having an end bead 18. This neck surrounds the running portion of the sleeve 12, and a pair of horizontal flanges 19, 20, bearing on the bead 18, crushes a joint ring 21 between the end edge of the neck 17 and the outer surface of the sleeve 12, by means of not shown bolts, to seal.
La cloche 14 (figure 3) comporte une tubulure laterale 22 traversée par le dispositif d'allumage 15, lequel est monté de façon amovible. Ce dispositif caqprend une plaque-support 23 présentant un orifice central et plaqué contre la tranche d'extremite de la tubulure 22, avec interposition d'un joint torique 24, par serrage de cette plaque, au moyen de boulons non représentés, vers une bride 25 qui prend appui sur un bourrelet d' extrémité 27 de la tubulure 22. Sur la face extérieure de la plaque 23 est fixée une rondelle dans laquelle se visse radialement une vis de guidage 28. The bell 14 (Figure 3) has a side pipe 22 through which the ignition device 15, which is removably mounted. This device comprises a support plate 23 having a central orifice and pressed against the end edge of the pipe 22, with the interposition of an O-ring 24, by clamping this plate, by means of bolts (not shown), towards a flange. 25 which is supported on an end bead 27 of the tubing 22. On the outer face of the plate 23 is fixed a washer in which is screwed radially a guide screw 28.
Du côté intérieur, un manchon de guidage 29 est fixé dans l'orifice de la plaque 23. Une tige 30 traverse avec un petit jeu la plaque 23 et le manchon 29. Cette tige porte à son extrémité extérieure un bouton de manoeuvre 31, présente dans sa partie médiane une rainure 32 coopérant avec -la pointe de la vis 28, et porte à son extrémité intérieure un embout isolant 33 équipé d'un pontet métallique 34 en forme de S. Un soufflet d'étanchéité 35 est fixé par une extrEnite à l'embout 33 et par son autre extrémité au manchon 29. Une butée réglable 36 est fixée sur la tige 30, à l'extérieur par rapport à la plaque 23. On the inner side, a guide sleeve 29 is fixed in the orifice of the plate 23. A rod 30 passes through a small clearance plate 23 and the sleeve 29. This rod carries at its outer end an operating knob 31, present in its middle part a groove 32 cooperating with -the tip of the screw 28, and carries at its inner end an insulating tip 33 equipped with a metal bridge 34 S-shaped. A sealing bellows 35 is fixed by an extrEnite at the tip 33 and at its other end to the sleeve 29. An adjustable stop 36 is fixed on the rod 30, outside with respect to the plate 23.
On comprend que la tige 30 peut être déplacée entre deux positions, représentées toutes deux sur la figure 3 : une position de repos, dans laquelle elle est tirée vers l'intérieur de la cloche et le pontet 34 est escamoté dans la tubulure 22, et une position active d'allumage du plasma. Dans cette position active, on a poussé la tige 30 vers l'intérieur de la cloche jusqu'à ce que la butée 36 soit arrêtée par la rondelle pourvue de la vis 28. Ce mouvement est guidé à peu près en translation par la vis 28 et la rainure 32, mais un jeu angulaire entre ces deux éléments, de l'ordre de 10 , ainsi que le petit jeu circonférentiel entre la tige 30 d'une part et le manchon 29 et l'orifice de la plaque 23 d'autre part, permettent d'amener l'extrémité du pontet 34 sous 1' extrémité des tubes 7 et 8, puis simultanément contre les tranches d'extrémité de ces deux tubes ; on crée ainsi un court-circuit provoquant 1 'allumage du plasma micro-onde, pourvu bien entendu que la torche soit à ce minent alimentée en gaz plasmagène et en énergie micro-onde (ou hyperfrequence). It is understood that the rod 30 can be moved between two positions, both shown in Figure 3: a rest position, in which it is pulled inwardly of the bell and the bridge 34 is retracted into the tubing 22, and an active ignition position of the plasma. In this active position, the rod 30 is pushed towards the inside of the bell until the stop 36 is stopped by the washer provided with the screw 28. This movement is guided approximately in translation by the screw 28. and the groove 32, but an angular clearance between these two elements, of the order of 10, and the small circumferential clearance between the rod 30 on the one hand and the sleeve 29 and the orifice of the plate 23 on the other part, allow to bring the end of the bridge 34 under one end of the tubes 7 and 8, and simultaneously against the end slices of these two tubes; a short-circuit is thus created causing the microwave plasma to ignite, provided of course that the torch is at this minute supplied with plasma gas and with microwave energy (or microwave).
La double enveloppe 16 comprend une partie supérieure cylindrique, une partie intermédiaire cylindrique de même diamètre et une partie inférieure conique convergente vers le bas et débouchant dans le dispositif collecteur 3. Son extrémité supérieure est appliquée contre la tranche d'extrémité inférieure de la cloche 14, qui présente le même diamètre intérieur, au moyen d'un serrage par brides et d'un joint d'étanchéité torique, de la même manière que la plaque 23 est fixée sur la tubulure 22. La double enveloppe 16 est pourvue, dans sa partie supérieure, d'orifices 37 d'injection d'un gaz de confinement, orientés tangentiellement, et d'orifices 38 d'injection d'un gaz de refroidissement.De chacun de ces derniers part une crosse 39 dont la partie courante monte le long de la paroi interne de l'enveloppe et pénètre dans la cloche 14 et dont la sortie, orientée vers le bas et légèrement inclinée vers l'axe X-X, débouche à une petite distance au-dessous de l'extrémite inférieure de la torche 1. De plus, la double enveloppe 16 comprend des moyens de refroidissement à l'eau, lesquels permettent à de l'eau de circuler en série de haut en bas dans les trois parties de cette enveloppe, entre une entre supérieure 40 et une sortie inférieure 41. En variante, l'eau pourrait circuler de bas en haut dans l'enveloppe 16. Dans cette dernière débouche encore une conduite latérale 42 équipée d'une page à vide 33 et d'une soupape 44 de régulation de pression. The jacket 16 comprises a cylindrical upper portion, a cylindrical intermediate portion of the same diameter and a lower conical bottom portion converging downwards and opening into the collecting device 3. Its upper end is applied against the lower end edge of the bell 14 , which has the same internal diameter, by means of a clamping flange and an O-ring seal, in the same way that the plate 23 is fixed on the tubing 22. The casing 16 is provided, in its upper part, orifices 37 for injecting a confinement gas, oriented tangentially, and orifices 38 for injecting a cooling gas. From each of these parts a butt 39, the current portion of which along the inner wall of the envelope and enters the bell 14 and whose outlet, oriented downwards and slightly inclined towards the axis XX, opens at a small distance below the lower end of the torch 1. In addition, the jacket 16 comprises water cooling means, which allow water to circulate in series from top to bottom in the three parts of this envelope, between an upper inlet 40 and a lower outlet 41. In a variant, the water could circulate upwardly in the enclosure 16. In the latter, a lateral pipe 42 equipped with a vacuum page 33 and a valve 44 of pressure regulation.
Le dispositif 3 peut être tout dispositif approprié de collection de poudre, par exemple un filtre. Une conduite 45 d'évacuation de l'effluent gazeux du réacteur mène de la sortie du dispositif 3 à une station non représentée de traitement de cet effluent. Les gaz de gainage, de confinement et de refroidissement sont des gaz inertes, de préférence de l'azote pour des raisons éconcmiques. Le gaz de refroidissement peut contenir une certaine proportion d'hélium pour en arrliorer la conductivité thermique. Le gaz plasmagène est de préférence de l'argon. The device 3 may be any appropriate powder collection device, for example a filter. A pipe 45 for evacuating the gaseous effluent from the reactor leads from the outlet of the device 3 to a not shown station for treating this effluent. Cladding, containment and cooling gases are inert gases, preferably nitrogen for economic reasons. The cooling gas may contain a certain proportion of helium to improve the thermal conductivity. The plasma gas is preferably argon.
L'appareil ainsi décrit fonctionne de la manière suivante. The apparatus thus described operates in the following manner.
On évacue d'abord de l'appareil l'air qu'il contient, au moyen de la pcmpe à vide 43, par exemple jusqu'à une pression de 11 ordre de 10 itrn Hg, puis on introduit de l'azote ou de l'argon jusqu'à obtenir une pression de l'ordre de 1,3 bar absolu. Après avoir éventuellement répété ces opérations préliminaires plusieurs fois, l'appareil se trouve sous atmosphère inerte, sous 1,3 bar, et ne contient plus ni oxygène ni eau. Pendant toute la suite du fonctionnement, la pression reste régulée à 1,3 bar dans l'enceinte 2 par la soupape 44, ce qui garantit l'absence de pénétration d'oxygène et d'humidité dans l'appareil. The air which it contains is first discharged from the apparatus by means of the vacuum pump 43, for example up to a pressure of 10 μm Hg, and then nitrogen or nitrogen is introduced. argon until a pressure of the order of 1.3 bar absolute. After possibly repeated these preliminary operations several times, the apparatus is under an inert atmosphere, under 1.3 bar, and contains no oxygen or water. Throughout the rest of the operation, the pressure remains regulated at 1.3 bar in the chamber 2 by the valve 44, which ensures the absence of oxygen and moisture penetration into the apparatus.
On envoie ensuite le gaz plasmagène et le gaz de gainage par les tubes 7 et 12, les gaz de confinement et de refroidissement par les orifices 37 et les crosses 39, l'énergie hyperfréquence par le guide d'onde 5 et l'embout 6, et on allume le plasma à l'extrémité aval de la torche au moyen du dispositif d'allumage 15 de la manière décrite plus haut. On obtient ainsi un jet de plasma annulaire à la sortie de la torche 1. On envoie alors le gaz réactif par le tube central 8. Ce gaz est traité thermiquement par le plasma en traversant celui-ci, et les produits de la réaction sont trempés par les jets de gaz de refroidissement sortant des crosses 39.Il se forme ainsi une poudre à fine granularétrie, que les jets tangentiels de gaz de confinement, qui décrivent des trajets hélicoidaux descendants, eschent de se déposer sur la paroi interne de 1 1enveloppe 16. La poudre est recueillie par le dispositif 3 et évacuée, en continu ou périodiquement suivant la nature de ce dispositif. The plasmagene gas and the cladding gas are then sent through the tubes 7 and 12, the confinement and cooling gases through the orifices 37 and the butts 39, the microwave energy through the waveguide 5 and the tip 6 and the plasma is turned on at the downstream end of the torch by means of the ignition device 15 in the manner described above. An annular plasma jet is thus obtained at the outlet of the torch 1. The reactive gas is then sent through the central tube 8. This gas is thermally treated by the plasma while passing through it, and the products of the reaction are quenched. by the jets of cooling gas leaving the sticks 39. A fine granularity powder is thus formed, that the tangential jets of confining gas, which describe descending helical paths, are intended to be deposited on the inner wall of the casing 16 The powder is collected by the device 3 and discharged, continuously or periodically according to the nature of this device.
A titre d'exemples d'utilisation de l'appareil, on peut citer
(a) des réactions de double décoposition en phase gazeuse, particulièrement intéressantes pour la fabrication de composés ou de revêtements réfractaires
As examples of use of the apparatus, mention may be made of
(a) Double-decoding reactions in the gas phase, of particular interest for the manufacture of refractory compounds or coatings
<tb> 3SiH4 <SEP> (silane) <SEP> + <SEP> 2N2 <SEP> ySi3N4 <SEP> (nitrure <SEP> de <SEP> silicium) <SEP> + <SEP> 6H2,
<tb>
une réaction analogue pouvant être cbtenue en revlaçant N2 par NH3 et/ou SiH4 par SiCl4.
<tb> 3SiH4 <SEP> (silane) <SEP> + <SEP> 2N2 <SEP> ySi3N4 <SEP> (nitride <SEP> from <SEP> silicon) <SEP> + <SEP> 6H2,
<Tb>
a similar reaction can be carried out by revolving N 2 with NH 3 and / or SiH 4 by SiCl 4.
<tb> SiH4 <SEP> + <SEP> CH4 <SEP> H <SEP> SiC <SEP> (carbure <SEP> de <SEP> silicium) <SEP> + <SEP> 4H2
<tb> B2H6 <SEP> + <SEP> N2 <SEP> > <SEP> 2BN <SEP> (nitrure <SEP> de <SEP> bore) <SEP> + <SEP> 3H2,
<tb>
une réaction analogue pouvant être obtenue en remplaçant N2 par
NH3 et/ou B2H6 par un autre composé du bore du type BX3.
(carbure de bore)
(borure de titane)
(nitrure de titane)
(carbure de titane),
ces dernières réactions n'étant bien entendu pas écrites sous forme équilibrée.<tb> SiH4 <SEP> + <SEP> CH4 <SEP> H <SEP> SiC <SEP> (carbide <SEP> of <SEP> silicon) <SEP> + <SEP> 4H2
<tb> B2H6 <SEP> + <SEP> N2 <SEP>><SEP> 2BN <SEP> (nitride <SEP> of <SEP> boron) <SEP> + <SEP> 3H2,
<Tb>
a similar reaction can be obtained by replacing N2 with
NH3 and / or B2H6 by another boron compound of the BX3 type.
(boron carbide)
(titanium boride)
(titanium nitride)
(titanium carbide),
these latter reactions are of course not written in balanced form.
(b) des réactions d'oxydation en phase gazeuse, destinées par exemple à la production de poudres d'oxydes de métaux rares tels que yttrium, scandium, vanadium, ruthénium. Ces oxydes, obtenus par oxydation des halogénures des marnes mstaux, servent notamnent de photo-émetteurs pour les écrans de télévision couleur. Les réactions sont du type
(b) gas phase oxidation reactions, for example for the production of rare metal oxide powders such as yttrium, scandium, vanadium, ruthenium. These oxides, obtained by oxidation of metal halide halides, serve in particular as photo-emitters for color television screens. The reactions are of the type
X désignant un atome d'halogène.X denotes a halogen atom.
De marne, on peut fabriquer de la poudre de silice amorphe submicronique, entrant dans la préparation des pâtes gingivales, par la réaction
From marl, we can manufacture submicron amorphous silica powder, used in the preparation of gum pasta, by the reaction
(c) des réactions de réduction, permettant par exemple de produire des poudres de métaux, par exenple
(c) reduction reactions, for example making it possible to produce metal powders, for example
Dans ce cas, on peut faire intervenir l'hydrogêne en mélange avec TiCl4 ou SiCl4, dans le tube central 8, et/ou carme composant d'un mélange gazeux plasmagène tel que argon-hydrogène. In this case, the hydrogen may be used in admixture with TiCl 4 or SiCl 4, in the central tube 8, and / or as a component of a plasmagene gas mixture such as argon-hydrogen.
(d) des réactions de simple déocoosition, conduisant par exemple à la production de poudres métalliques, par exemple
SiH4 > Si + 2H2.(d) reactions of simple deocoosition, leading for example to the production of metal powders, for example
SiH4> Si + 2H2.
Dans ce cas, le gaz réactif n'est pas un mélange canne dans les exemples précédents, mais est constitué par le corps decomposé thermiquement (SiH4 dans cet exemple).In this case, the reactive gas is not a cane mixture in the previous examples, but is constituted by the thermally decomposed body (SiH4 in this example).
Plus généralement, l'invention s'applique à la fabrication de poudres suumicroniques de nanbreux matériaux tels que des métaux, des céramiques ou des oxydes, à partir d'un corps ou de plusieurs corps gazeux à une température peu éloignée de la température arrbiante par rapport aux temperatures atteintes dans un plasma micro-onde, c'est-à-dire comprise entre la température ambiante et quelques centaines de degrés Celsius. More generally, the invention is applicable to the manufacture of suumicron powders of many materials such as metals, ceramics or oxides, from a body or of several gaseous bodies at a temperature not far from the bending temperature by relative to the temperatures reached in a microwave plasma, that is to say between room temperature and a few hundred degrees Celsius.
La haute qualité des poudres ainsi cbtenues permet de les utiliser pour fabriquer des pièces ayant des structures métalliques à grains très fins, et donc possédant d'exellentes propriétés irecaniques, ou encore pour réaliser des revêtements de surface d'épaisseur très faible par dépôt ou projection. On remarque que la pureté des corps obtenus depend uniquement de celle des gaz utilisés, puisque l'appareil est entièrement isolé de l'atmosphère environnante. The high quality of the powders thus obtained makes it possible to use them to manufacture parts having very fine-grained metal structures, and therefore possessing excellent irecanic properties, or even for producing surface coatings of very small thickness by deposition or spraying. . It is noted that the purity of the bodies obtained depends solely on that of the gases used, since the apparatus is entirely isolated from the surrounding atmosphere.
Dans une variante non représentée, le tube 7 de la torche 1 est supprimé, et l'on envoie dans l'unique tube 8 à la fois le gaz plasmagène et le gaz réactif. On peut également envisager d'envoyer le gaz réactif à travers le plasma à partir d'un emplacement de 1 'enceinte 2 extérieur à la torche. In a variant not shown, the tube 7 of the torch 1 is removed, and is sent into the single tube 8 at a time the plasma gas and the reactive gas. It is also conceivable to send the reactive gas through the plasma from a location of the enclosure 2 outside the torch.
Claims (15)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8518240A FR2591412A1 (en) | 1985-12-10 | 1985-12-10 | Method for the production of powders and a sealed microwave plasma reactor |
JP61292634A JPS62152532A (en) | 1985-12-10 | 1986-12-10 | Method for producing powder and hermetically closed microwave plasma reactor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8518240A FR2591412A1 (en) | 1985-12-10 | 1985-12-10 | Method for the production of powders and a sealed microwave plasma reactor |
Publications (1)
Publication Number | Publication Date |
---|---|
FR2591412A1 true FR2591412A1 (en) | 1987-06-12 |
Family
ID=9325609
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
FR8518240A Withdrawn FR2591412A1 (en) | 1985-12-10 | 1985-12-10 | Method for the production of powders and a sealed microwave plasma reactor |
Country Status (2)
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JP (1) | JPS62152532A (en) |
FR (1) | FR2591412A1 (en) |
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EP0313980A1 (en) * | 1987-10-23 | 1989-05-03 | AeroChem Research Laboratories, Inc. | Process and apparatus for the preparation of ceramic powders |
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EP0334791A1 (en) * | 1988-03-24 | 1989-09-27 | Union Explosivos Rio Tinto, S.A. | Process for the preparation of silicon nitride |
FR2630427A1 (en) * | 1988-04-23 | 1989-10-27 | Tioxide Group Plc | BLACK POWDER OF TITANIUM NITRIDE AND METHOD OF MANUFACTURING THE SAME |
EP0421314A1 (en) * | 1989-10-02 | 1991-04-10 | Phillips Petroleum Company | Carbide products and method and apparatus for their production |
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