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EP0296921A1 - Microwave plasma torch, device comprising such a torch and production procedure for powder operating them - Google Patents

Microwave plasma torch, device comprising such a torch and production procedure for powder operating them Download PDF

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Publication number
EP0296921A1
EP0296921A1 EP88401405A EP88401405A EP0296921A1 EP 0296921 A1 EP0296921 A1 EP 0296921A1 EP 88401405 A EP88401405 A EP 88401405A EP 88401405 A EP88401405 A EP 88401405A EP 0296921 A1 EP0296921 A1 EP 0296921A1
Authority
EP
European Patent Office
Prior art keywords
gas
sleeve
waveguide
pipe
coaxial
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP88401405A
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German (de)
French (fr)
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EP0296921B1 (en
Inventor
Jean-Luc Labat
Lahcen Ougarane
Michel Gastiger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP0296921A1 publication Critical patent/EP0296921A1/en
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Publication of EP0296921B1 publication Critical patent/EP0296921B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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
    • H05H1/26—Plasma torches
    • H05H1/30—Plasma torches using applied electromagnetic fields, e.g. high frequency or microwave energy
    • 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

Definitions

  • the present invention relates to a microwave plasma torch as well as a device and a method for the manufacture of powder using such a torch.
  • the present invention relates to a microwave plasma torch characterized in that it comprises at least one gas supply pipe; a resonant cavity forming around said pipe a sleeve open on the side of the outlet of said pipe and comprising a lateral opening; a coaxial transition structure perpendicular to the sleeve comprising on the one hand an external tube connected to the lateral opening of the sleeve and on the other hand an internal member one end of which is in contact with said pipe and the other end of which is in contact with the internal face of a waveguide and carries a transition piece disposed in the waveguide; said microwave power supply waveguide of rectangular section and perpendicular to the coaxial structure being provided with an opening where the outer tube of said structure is connected; cladding gas supply means in the waveguide and / or the coaxial structure and / or the sleeve; possibly means of agreement; and possibly plasma ignition means.
  • FIGS. 1, 2 and 3 a coaxial gas supply pipe appears, the internal pipe 1 conducting the active gas introduced by the end 22 connected to a gas source, not shown. Via the transverse pipe 23 connected to a source of plasma gas not shown, the gas circulating in the outside pipe 2 arrives conductive material.
  • the coaxial pipe (1,2) is surrounded by a cylindrical metallic sleeve of the same axis forming a resonance cavity 3 closed on the side of the gas inlet by an annular flange 18 fixed on the sleeve 3 by screws 19. This flange 18 is traversed by and screwed onto the hollow rod and externally threaded with a piston 9 sliding in the sleeve 3 and taken through the pipe 1,2.
  • O-rings 25, 25 ′, 26 and 26 ′ ensure gas tightness.
  • the sleeve 3 has a lateral opening 4 on which the metallic external tube 5 of the coaxial transition structure is fixed perpendicularly to the gasket.
  • the internal metallic member 6 disposed on the axis of the coaxial structure is on the one hand in contact with the external pipe 2, the contact being produced by a removable contact piece 20 and on the other hand in contact with the internal face of the wall of the waveguide of rectangular section 8 opposite to the circular opening 27 where the outer tube 5 of the coaxial structure is connected with a gasket.
  • the waveguide 8 is arranged perpendicular to the coaxial structure and to the axis of the pipe and of the sleeve 3.
  • the internal member 6 is provided with a piece 7 of agreement which is not necessarily fixed.
  • the waveguide 8 opens a pipe 21 for supplying sheathing gas.
  • the sleeve-forming cavity 3 is extended by the sleeve 10 disposed around the pipe 1,2 and which carries a fixing flange 17.
  • the central portions 24 and the lateral portions 23-23 ′ also appear on the waveguide 8, the double flanges 12-13 fixed between the flanges 28 and 29 integral with portions 23-23′ and 24 respectively. waveguide 8.
  • the window structure appears, each comprising two rectangular metal flanges 12 and 13 which enclose in a recess 15 a window 11 transparent to waves, for example made of quartz.
  • the flange 13 further has a groove and 16 where is disposed a rectangular metal gasket which seals the central portion 24 of the waveguide 8 with gas by contact on the flange 28.
  • edges and the sharp angles are softened to avoid the arcing of the plasma.
  • the flange 18 is crossed in its center only by the line 1,2 and the piston 9, inside the sleeve and without a hollow rod, is moved into the sleeve by one or more rods passing through the flange 18 .
  • the introduction of sheathing gas takes place in the sleeve 3 or 10.
  • the gas tightness in the torch can be ensured by a part arranged in the coaxial structure for example, the windows 12, 13 are then not necessary.
  • gas sealing means are not necessary in certain applications of these torches.
  • the coaxiality of the pipes 1 and 2 is ensured by means of pins or a metal spring disposed between the two pipes.
  • the gas supply line is not necessarily coaxial and may consist of only one line.
  • the length of lines 1 and 2 can be changed in line by sliding along the axis. These lengths and that of the sleeve can be further modified by the addition of end caps 30,31,32 screwed at their end and interchangeable.
  • these tips can be chosen from a material suitable for the products treated in the torch, good conductors with a high melting point and preferably refractory for the sleeve and the outer pipe, possibly also refractory for the pipe 1 and not necessarily conductive.
  • the end of the pipes 1,2 and of the sleeve 10 or of the end caps screwed at their end is rounded.
  • the present invention also relates to a sealed device for the manufacture of powder which uses a torch according to the invention and further comprises a microwave generator, a microwave plasma torch, a reaction vessel, supply means. reactive gas, plasma gas and a cladding gas, means for separation of powder and gases, means for collecting powders, and means for discharging effluent gases.
  • the device comprises a microwave generator 41 connected by usual means to the waveguide 48. It also includes pipes for supplying sheathing gas 42, reactive gas 47 and plasma gas 46. Means of tuning, for example pistons can be provided on the waveguide. Other usual means of agreement are also possible.
  • the sleeve 40 opens and protrudes from D1 into the reaction vessel 53 of length L and of diameter D, the end opposite to a cone shape with an angle preferably approximately equal to 20 °.
  • the L / D ratio is between 1.5 and 6, preferably between 2 and 4.
  • the enclosure wall To avoid contamination of the powders by the material of the enclosure wall, it can be electropolished or fitted with a quartz lining.
  • the reaction chamber opens into a powder and gas separator consisting of a metallic cylindrical filter 50 surrounded by a sealed sleeve 49 and connected to a gas evacuation pipe 52.
  • a powder collector 51 valves and a supply 56 of purge gas and a vacuum line 55 are further provided to facilitate the change of collector without contamination of the powders.
  • Other usual means for separating powder and gas can be envisaged.
  • the ignition device 54 allows the plasma to be ignited by electrical contact with the gas line.
  • the plasma ignition means are not necessarily chosen as shown. They can be constituted by any usual ignition means at the end of the pipe, by any external means compatible with the structure of the enclosure. It can in particular be produced by means of a metal wire introduced into the pipe 2 and removable or not once the plasma is on.
  • the cladding gas can be introduced at the sleeve 40 or the cavity 43 or the coaxial (which does not appear in FIG. 5) and the plasma gas by the internal organ of the coaxial transition which in this case leads into the external pipe 2 to lead the plasma gas there.
  • the torch in which the gases in the configuration shown here circulate from top to bottom can be oriented in a different way, for example oriented from bottom to top.
  • the device according to the invention applies in particular to the synthesis of powder, this is why the present invention also relates to a process for the preparation of powder, characterized in that a device according to the invention is used and in that the reactive gas is chosen from silanes, ammonia, boron hydrides, tungsten and titanium halides, oxygen and gaseous organo-metals and their mixtures.
  • the method according to the invention applies in particular to the preparation of silicon-based powder, namely silicon, silica, carbide and silicon nitride powder.
  • the reactive gas is then according to the invention chosen from silanes and polysilanes, halogenosilanes, alkylsilanes and their mixture with oxygen and ammonia.
  • the cladding gas ultimately flows, regardless of the supply line, between the sleeve and the external pipe 2.
  • Any conventional cladding gas can be used, and in particular inert gases such as nitrogen or hydrogen for example.
  • the plasma gas used is a conventional plasma gas, in particular argon.
  • the active gas circulates in the internal pipe or in the single pipe when this embodiment is used.
  • plamagen gas can be injected at ignition and then replaced by or mixed with active gas.
  • the resumption of use is of the order of atmospheric pressure or higher than this, up to approximately 5 atmosphere.
  • microwave By microwave is meant the band from about 400 to 12000 MHz.
  • - L / D 2.5; D1 between D / 4 and 3 D / 4, preferably 0.4 D.
  • - D / d1 between 40 and 150, preferably 100.
  • - d1 2 mm (internal diameter of pipe 1)
  • - d2 4 mm (external diameter of pipe 1)
  • - d3 7.5 mm (internal diameter of pipe 2)
  • - d4 12 mm (external diameter of pipe 2)
  • - d5 27 mm (internal diameter of the sleeve 10)
  • - d6 33 mm (external diameter of the sleeve 10)
  • - line 1 has a quartz tip - line 2 has a tungsten tip - sleeve 10 has a brass tip -
  • the reactor is made of 316 L stainless steel - (the internal reference temperature is 440 ° C).
  • a single crystal was drawn from the powders thus obtained. Analysis of the single crystal revealed 7 1017 atom / cm3 of oxygen and 10 1017 atom / cm3 of carbon.
  • the diameters d1 to d6 are defined in Figure 1.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Electromagnetism (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Plasma Technology (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

Microwave plasma torch characterised in that it comprises at least one gas-intake duct (1, 2); a resonator cavity (3) forming, around the said duct, a sleeve open on the exit side of the said duct and comprising a lateral opening (4); a coaxial transition structure perpendicular to the sleeve comprising on the one hand an outer tube (5) connected to the lateral opening (4) of the sleeve and on the other hand an inner member (6) one of whose ends (20) is in contact with the said duct and whose other end is in contact with the outer surface of a waveguide (8) and carries a transition piece (7) disposed inside the waveguide (8); the said waveguide (8) for supplying microwave energy with rectangular cross-section and perpendicular to the coaxial structure (5, 6) being provided with an opening (27) wherein is connected the outer tube (5) of the said structure; means of supplying cladding gas in the waveguide (8) and/or the coaxial structure (5, 6) and/or the sleeve; possibly tuning means; and possibly means of igniting the plasma. <??>It also relates to a device and a method for manufacturing powder. <IMAGE>

Description

La présente invention concerne une torche à plasma micro-onde ainsi qu'un dispositif et un procédé pour la fabrication de poudre mettant en oeuvre une telle torche.The present invention relates to a microwave plasma torch as well as a device and a method for the manufacture of powder using such a torch.

Il est connu de préparer des poudres par réaction de gaz réactifs au sein d'un plasma, ces procédés consomment cependant en général trop d'énergie.It is known to prepare powders by reacting reactive gases within a plasma, these methods however generally consume too much energy.

La présente invention concerne une torche à plasma micro-onde caractérisé en ce qu'elle comporte au moins une conduite d'amenée de gaz ; une cavité résonnante formant autour de ladite conduite un manchon ouvert du coté de la sortie de ladite conduite et comportant une ouverture latérale ; une structure coaxiale de transition perpendiculaire au manchon comportant d'une part un tube externe raccordé à l'ouverture latérale du manchon et d'autre part un organe interne dont l'une des extrémités est au contact de ladite conduite et dont l'autre extrémité est au contact de la face interne d'un guide d'onde et porte une pièce de transition disposée dans le guide d'ondes ; ledit guide d'onde d'alimentation en énergie micro-ondes à section rectangulaire et perpendiculaire à la structure coaxiale étant pourvue d'une ouverture où est raccordé le tube externe de ladite structure ; des moyens d'alimentation en gaz de gainage dans le guide d'onde et/ou la structure coaxiale et/ou le manchon ; éventuellement des moyens d'accord ; et éventuellement des moyens d'allumage du plasma.The present invention relates to a microwave plasma torch characterized in that it comprises at least one gas supply pipe; a resonant cavity forming around said pipe a sleeve open on the side of the outlet of said pipe and comprising a lateral opening; a coaxial transition structure perpendicular to the sleeve comprising on the one hand an external tube connected to the lateral opening of the sleeve and on the other hand an internal member one end of which is in contact with said pipe and the other end of which is in contact with the internal face of a waveguide and carries a transition piece disposed in the waveguide; said microwave power supply waveguide of rectangular section and perpendicular to the coaxial structure being provided with an opening where the outer tube of said structure is connected; cladding gas supply means in the waveguide and / or the coaxial structure and / or the sleeve; possibly means of agreement; and possibly plasma ignition means.

La présente invention sera mieux comprise au regard des figures annexées sur lesquels :

  • - la figure 1 représente une coupe latérale d'une torche selon l'invention dans son plan de symétrie ;
  • - la figure 2 représente une vue de face de la torche ;
  • - la figure 3 représente une vue de dessus de la torche ;
  • - la figure 4 représente une vue en coupe de la fenêtre d'étanchéité au gaz ;
  • - la figure 5 représente une vue schématique d'un dispositif selon l'invention.
The present invention will be better understood with reference to the appended figures in which:
  • - Figure 1 shows a side section of a torch according to the invention in its plane of symmetry;
  • - Figure 2 shows a front view of the torch;
  • - Figure 3 shows a top view of the torch;
  • - Figure 4 shows a sectional view of the gas-tight window;
  • - Figure 5 shows a schematic view of a device according to the invention.

Sur les figures 1,2 et 3 apparait une conduite coaxiale d'amenée de gaz, la conduite intérieure 1 conduisant le gaz actif introduit par l'extrémité 22 reliée à une source de gaz non représentée. Par la conduite transversale 23 reliée à une source de gaz plasmagène non représenté arrive le gaz circulant dans la conduite extérieure 2 en matériau conducteur. La conduite coaxiale (1,2) est entourée d'un manchon métallique cylindrique de même axe faisant cavité de resonnance 3 fermée du coté de l'arrivée des gaz par une bride 18 annulaire fixée sur le manchon 3 par des vis 19. Cette bride 18 est traversée par et vissée sur la tige creuse et extérieurement filetée d'un piston 9 coulissant dans le manchon 3 et empruntée par la conduite 1,2. Des joints 25, 25′, 26 et 26′ toriques assurent l'étanchéité aux gaz.In FIGS. 1, 2 and 3, a coaxial gas supply pipe appears, the internal pipe 1 conducting the active gas introduced by the end 22 connected to a gas source, not shown. Via the transverse pipe 23 connected to a source of plasma gas not shown, the gas circulating in the outside pipe 2 arrives conductive material. The coaxial pipe (1,2) is surrounded by a cylindrical metallic sleeve of the same axis forming a resonance cavity 3 closed on the side of the gas inlet by an annular flange 18 fixed on the sleeve 3 by screws 19. This flange 18 is traversed by and screwed onto the hollow rod and externally threaded with a piston 9 sliding in the sleeve 3 and taken through the pipe 1,2. O-rings 25, 25 ′, 26 and 26 ′ ensure gas tightness.

Le manchon 3 comporte une ouverture latérale 4 sur laquelle est fixée perpendiculairement à joint étanche le tube externe métallique 5 de la structure de transition coaxiale. L'organe interne métallique 6 disposée sur l'axe de la structure coaxiale est d'une part au contact de la conduite externe 2, le contact étant réalisé par une pièce de contact 20 amovible et d'autre part au contact de la face interne de la paroi du guide d'ondes à section rectangulaire 8 opposée à l'ouverture 27 circulaire où est raccordée à joint étanche le tube externe 5 de la structure coaxiale. Le guide d'onde 8 est disposé perpendiculairement à la structure coaxiale et à l'axe de la conduite et du manchon 3. L'organe interne 6 est pourvu d'une pièce 7 d'accord non nécessairement fixe.The sleeve 3 has a lateral opening 4 on which the metallic external tube 5 of the coaxial transition structure is fixed perpendicularly to the gasket. The internal metallic member 6 disposed on the axis of the coaxial structure is on the one hand in contact with the external pipe 2, the contact being produced by a removable contact piece 20 and on the other hand in contact with the internal face of the wall of the waveguide of rectangular section 8 opposite to the circular opening 27 where the outer tube 5 of the coaxial structure is connected with a gasket. The waveguide 8 is arranged perpendicular to the coaxial structure and to the axis of the pipe and of the sleeve 3. The internal member 6 is provided with a piece 7 of agreement which is not necessarily fixed.

Dans le guide d'onde 8 débouche une canalisation 21 d'amenée de gaz de gainage. La cavité formant manchon 3 est prolongée par le manchon 10 disposé autour de la conduite 1,2 et qui porte une bride 17 de fixation.In the waveguide 8 opens a pipe 21 for supplying sheathing gas. The sleeve-forming cavity 3 is extended by the sleeve 10 disposed around the pipe 1,2 and which carries a fixing flange 17.

Sur la figure 2 apparait en outre sur le guide d'onde 8 les portions centrale 24 et les portions latérales 23-23′, les doubles brides 12-13 fixées entre les brides 28 et 29 solidaires respectivement des portions 23-23′et 24 du guide d'onde 8.In FIG. 2, the central portions 24 and the lateral portions 23-23 ′ also appear on the waveguide 8, the double flanges 12-13 fixed between the flanges 28 and 29 integral with portions 23-23′ and 24 respectively. waveguide 8.

Sur la figure 4 apparait la structure de fenêtres comportant chacune deux brides 12 et 13 rectangulaires metalliques qui enserrent dans une évidement 15 une fenêtre 11 transparente aux ondes, par exemple en quartz.In FIG. 4, the window structure appears, each comprising two rectangular metal flanges 12 and 13 which enclose in a recess 15 a window 11 transparent to waves, for example made of quartz.

L'étanchéité en gaz est assurée par des joints 14 en silicone disposés entre la fenêtre 11 et les surfaces en regard de la bride 12 et de l'évidement de la bride 13. La bride 13 comporte en outre une gorge et 16 où est disposé un joint rectangulaire métallique qui assure l'étanchéité au gaz de la portion centrale 24 du guide d'onde 8 par contact sur la bride 28.Gas tightness is ensured by silicone seals 14 disposed between the window 11 and the facing surfaces of the flange 12 and the recess of the flange 13. The flange 13 further has a groove and 16 where is disposed a rectangular metal gasket which seals the central portion 24 of the waveguide 8 with gas by contact on the flange 28.

De préférence, les arêtes et les angles vifs sont adoucis pour éviter l'arcage du plasma.Preferably, the edges and the sharp angles are softened to avoid the arcing of the plasma.

Dans une variante non représentée, la bride 18 n'est traversée en son centre que par la conduite 1,2 et le piston 9, intérieur au manchon et sans tige creuse, est déplacé dans le manchon par une ou plusieurs tiges traversant la bride 18.In a variant not shown, the flange 18 is crossed in its center only by the line 1,2 and the piston 9, inside the sleeve and without a hollow rod, is moved into the sleeve by one or more rods passing through the flange 18 .

Dans une autre variante non représentée, l'introduction de gaz de gainage a lieu dans le manchon 3 ou 10. L'étanchéité au gaz dans la torche peut être assurée par une pièce disposée dans la structure coaxiale par exemple, le fenêtres 12, 13 ne sont alors par nécessaires.In another variant not shown, the introduction of sheathing gas takes place in the sleeve 3 or 10. The gas tightness in the torch can be ensured by a part arranged in the coaxial structure for example, the windows 12, 13 are then not necessary.

En outre, les moyens d'étanchéité au gaz ne sont pas nécessaires dans certaines applications de ces torches.In addition, the gas sealing means are not necessary in certain applications of these torches.

Est nécessaire par contre, un bon contact électrique entre toutes les parties conductrices qui guident les micro-ondes. A cet effet, leur jonction parfaitement conductrice entre les parties métalliques jointes par brides peut être assurée par des joints en cuivre ou en indium.On the other hand, a good electrical contact is necessary between all the conductive parts which guide the microwaves. To this end, their perfectly conductive junction between the metal parts joined by flanges can be ensured by copper or indium seals.

Dans une variante non représentée, la coaxialité des conduites 1 et 2 est assurée au moyen de picots ou d'un ressort métallique disposé entre les deux conduites.In a variant not shown, the coaxiality of the pipes 1 and 2 is ensured by means of pins or a metal spring disposed between the two pipes.

La conduite d'amenée de gaz n'est pas nécessairement coaxiale et peut n'être constituée que d'une conduite.The gas supply line is not necessarily coaxial and may consist of only one line.

La longueur des conduites 1 et 2 peut-être modifiée en ligne par coulissement le long de l'axe. Ces longueurs et celle du manchon peuvent être en outre modifiées par l'adjonction d'embouts 30,31,32 vissés à leur extrémité et interchangeables.The length of lines 1 and 2 can be changed in line by sliding along the axis. These lengths and that of the sleeve can be further modified by the addition of end caps 30,31,32 screwed at their end and interchangeable.

Selon l'application de la torche, ces embouts peuvent être choisis dans un matériau adapté aux produits traités dans la torche, bon conducteurs à point de fusion élevé et de préférence réfractaire pour le manchon et la conduite extérieure, éventuellement aussi réfractaire pour la conduite 1 et non néecessairement conducteur.Depending on the application of the torch, these tips can be chosen from a material suitable for the products treated in the torch, good conductors with a high melting point and preferably refractory for the sleeve and the outer pipe, possibly also refractory for the pipe 1 and not necessarily conductive.

De préférence, l'extrémité des conduites 1,2 et du manchon 10 ou des embouts vissés à leur extrémité est arrondie.Preferably, the end of the pipes 1,2 and of the sleeve 10 or of the end caps screwed at their end is rounded.

La présente invention concerne également en dispositif étanche pour la fabrication de poudre qui met en oeuvre une torche selon l'invention et comporte en outre un générateur micro-ondes, une torche à plasma micro-ondes, une enceinte réactionnelle, des moyens d'alimentation en gaz réactif, en gaz plasmagène et un gaz de gainage, des moyens de séparation de poudre et des gaz, des moyens de collection des poudres, et des moyens d'évacuation des gaz effluents.The present invention also relates to a sealed device for the manufacture of powder which uses a torch according to the invention and further comprises a microwave generator, a microwave plasma torch, a reaction vessel, supply means. reactive gas, plasma gas and a cladding gas, means for separation of powder and gases, means for collecting powders, and means for discharging effluent gases.

Outre la cavité de résonnance 43, le manchon 40 et le guide d'onde 48 qui correspondent à la cavité 3, au manchon 10 et au guide d'onde 8 représentés que les figures précédentes, le dispositif comporte un générateur de micro-ondes 41 relié par des moyens usuels au guide d'onde 48. Il comporte aussi des canalisations d'amenée de gaz de gainage 42, de gaz réactif 47 et de gaz plasmagène 46. Des moyens d'accord, par exemple des pistons peuvent être prévus sur le guide d'onde. D'autres moyens d'accord usuels sont également envisageables.In addition to the resonance cavity 43, the sleeve 40 and the waveguide 48 which correspond to the cavity 3, to the sleeve 10 and to the waveguide 8 shown in the preceding figures, the device comprises a microwave generator 41 connected by usual means to the waveguide 48. It also includes pipes for supplying sheathing gas 42, reactive gas 47 and plasma gas 46. Means of tuning, for example pistons can be provided on the waveguide. Other usual means of agreement are also possible.

Le manchon 40 débouche et dépasse de D₁ dans l'enceinte réactionnelle 53 de longueur L et de diamètre D, dont l'extrémité opposée à une forme de cône d'angle de préférence environ égal à 20°.The sleeve 40 opens and protrudes from D₁ into the reaction vessel 53 of length L and of diameter D, the end opposite to a cone shape with an angle preferably approximately equal to 20 °.

Selon l'invention, le rapport L/D est compris entre 1,5 et 6, de préférence entre 2 et 4.According to the invention, the L / D ratio is between 1.5 and 6, preferably between 2 and 4.

Pour éviter la contamination des poudres par le matériau de la parroi de l'enceinte, celle-ci peut être électropolie ou équipée d'une doublure en quartz.To avoid contamination of the powders by the material of the enclosure wall, it can be electropolished or fitted with a quartz lining.

L'enceinte réactionnelle débouche dans un séparateur de poudre et de gaz constitué d'un filtre cylindrique métallique 50 entouré d'un manchon 49 étanche et relié à une conduite d'évacuation des gaz 52. A la sortie du filtre cylindrique 50 est disposé un collecteur de poudre 51 des vannes et une alimentation 56 de gaz de purge et une conduite de mise sous vide 55 sont en outre prévues pour faciliter le changement de collecteur sans contamination des poudres. D'autres moyens usuels de séparation de poudre et de gaz sont envisageables.The reaction chamber opens into a powder and gas separator consisting of a metallic cylindrical filter 50 surrounded by a sealed sleeve 49 and connected to a gas evacuation pipe 52. At the outlet of the cylindrical filter 50 is disposed a powder collector 51 valves and a supply 56 of purge gas and a vacuum line 55 are further provided to facilitate the change of collector without contamination of the powders. Other usual means for separating powder and gas can be envisaged.

Le dispositif d'allumage 54 permet d'allumer le plasma par contact électrique avec la conduite de gaz.The ignition device 54 allows the plasma to be ignited by electrical contact with the gas line.

Le moyens d'allumage du plasma ne sont pas nécessairement choisi tels que représentés. Ils peuvent être constitués par tout moyen d'allumage usuel au niveau de l'extrémité de la conduite, par tout moyen extérieur compaptible avec la structure de l'enceinte. Il peut être en particulier réalisé au moyen d'un fil métallique introduit dans la conduite 2 et amovible ou non une fois le plasma allumé.The plasma ignition means are not necessarily chosen as shown. They can be constituted by any usual ignition means at the end of the pipe, by any external means compatible with the structure of the enclosure. It can in particular be produced by means of a metal wire introduced into the pipe 2 and removable or not once the plasma is on.

Dans un autre mode de réalisation non représenté, le gaz de gainage peut être introduit au niveau du manchon 40 ou de la cavité 43 ou du coaxial (qui n'apparait pas sur la figure 5) et le gaz plasmagène par l'organe interne de la transition coaxiale qui débouche dans ce cas dans la conduite externe 2 pour y conduire le gaz plasmagène.In another embodiment not shown, the cladding gas can be introduced at the sleeve 40 or the cavity 43 or the coaxial (which does not appear in FIG. 5) and the plasma gas by the internal organ of the coaxial transition which in this case leads into the external pipe 2 to lead the plasma gas there.

Dans un autre mode de réalisation, on peut prévoir d'autres modes usuels de récupération des poudres et des gaz à la sortie de l'enceinte réactionnelle. Les gaz résiduels peuvent être séparés, détruits pour certains toxiques et recyclés pour d'autres (plasmagène, de gainage).In another embodiment, other usual methods of recovering powders and gases can be provided at the outlet of the reaction vessel. Residual gases can be separated, destroyed for some toxic and recycled for others (plasmagenic, cladding).

Dans un autre mode de fonctionnement, la torche dans lesquels les gaz dans la configuration représenté ici circulent du haut vers le bas, peut être orientée de façon différente, par exemple orientée du bas vers le haut.In another operating mode, the torch in which the gases in the configuration shown here circulate from top to bottom, can be oriented in a different way, for example oriented from bottom to top.

Le dispositif selon l'invention s'applique notamment à la synthèse de poudre, c'est pourquoi la présente invention concerne également un procédé pour la préparation de poudre caractérisé en ce que l'on utilise un dispositif selon l'invention et en ce que le gaz réactif est choisi parmi les silanes, l'ammoniac, les hydrures de bore, les halogènures de tungstène et de titane, l'oxygène et les organo métalliques gazeux et leurs mélanges.The device according to the invention applies in particular to the synthesis of powder, this is why the present invention also relates to a process for the preparation of powder, characterized in that a device according to the invention is used and in that the reactive gas is chosen from silanes, ammonia, boron hydrides, tungsten and titanium halides, oxygen and gaseous organo-metals and their mixtures.

Le procédé selon l'invention s'applique en particulier à la préparation de poudre à base de silicium, à savoir poudre de silicium, de silice, de carbure et nitrure de silicium.The method according to the invention applies in particular to the preparation of silicon-based powder, namely silicon, silica, carbide and silicon nitride powder.

Le gaz réactif est alors selon l'invention choisi parmi les silanes et polysilanes, halogeno silanes, alkylsilanes et leur mélange à l'oxygène et à l'ammoniac.The reactive gas is then according to the invention chosen from silanes and polysilanes, halogenosilanes, alkylsilanes and their mixture with oxygen and ammonia.

Le gaz de gainage circule in fine, où que soit la conduite d'alimentation, entre le manchon et la conduite externe 2. On peut utiliser tout gaz de gainage usuel, et en particulier des gaz inertes comme l'azote, ou l'hydrogène par exemple.The cladding gas ultimately flows, regardless of the supply line, between the sleeve and the external pipe 2. Any conventional cladding gas can be used, and in particular inert gases such as nitrogen or hydrogen for example.

Le gaz plasmagène utilisé est un gaz plasmagène classique, en particulier l'argon.The plasma gas used is a conventional plasma gas, in particular argon.

Il est injecté et circule dans la conduite extérieure. Le gaz actif circule dans la conduite interne ou dans la conduite unique quand ce mode de réalisation est utilisé. Dans ce cas, du gaz plamagène peut être injecté à l'allumage puis remplacé par ou mélangé à du gaz actif.It is injected and circulates in the external pipe. The active gas circulates in the internal pipe or in the single pipe when this embodiment is used. In this case, plamagen gas can be injected at ignition and then replaced by or mixed with active gas.

Selon l'invention, la ression d'utilisation est de l'ordre de la pression atmosphérique ou supérieur à celle-ci, jusqu'à 5 atmosphère environ.According to the invention, the resumption of use is of the order of atmospheric pressure or higher than this, up to approximately 5 atmosphere.

Par micro-onde, on entend la bande allant d'environ 400 à 12000 MHz.By microwave is meant the band from about 400 to 12000 MHz.

Exemple 1.Example 1.

La demanderesse a mis en oeuvre l'invention dans les conditions suivantes :
- L/D = 2,5 ; D₁ compris entre D/4 et 3 D/4, de préférence 0,4 D.
- D/d₁ = compris entre 40 et 150, de préférence 100.
- d₁ = 2 mm (diamètre interne de la conduite 1)
- d₂ = 4 mm (diamètre externe de la conduite 1)
- d₃ = 7,5 mm (diamètre interne de la conduite 2)
- d₄ = 12 mm (diamètre externe de la conduite 2)
- d₅ = 27 mm (diamètre interne du manchon 10)
- d₆ = 33 mm (diamètre externe du manchon 10)
- la conduite 1 a un embout en quartz
- la conduite 2 a un embout en tungstène
- le manchon 10 a un embout en laiton
- le réacteur est en inox 316 L - (la température de référence interne est 440°C).
- gaz réactif : SiH₄      7l/mn
- gaz plasmagène : Ar      3l/mn
- gaz de gainage : N₂      11l/mn
- puissance µ-onde 2,5 Kw
- production = 490 g/h de poudre de silicium soit un rendement énergétique de 5,15 Kwh/kg de poudre et 7,90 KWh électrique/kg de poudre (conversion 100%, rendement ou générateur 66%).The applicant has implemented the invention under the following conditions:
- L / D = 2.5; D₁ between D / 4 and 3 D / 4, preferably 0.4 D.
- D / d₁ = between 40 and 150, preferably 100.
- d₁ = 2 mm (internal diameter of pipe 1)
- d₂ = 4 mm (external diameter of pipe 1)
- d₃ = 7.5 mm (internal diameter of pipe 2)
- d₄ = 12 mm (external diameter of pipe 2)
- d₅ = 27 mm (internal diameter of the sleeve 10)
- d₆ = 33 mm (external diameter of the sleeve 10)
- line 1 has a quartz tip
- line 2 has a tungsten tip
- sleeve 10 has a brass tip
- the reactor is made of 316 L stainless steel - (the internal reference temperature is 440 ° C).
- reactive gas: SiH₄ 7l / min
- plasma gas: Ar 3l / min
- cladding gas: N₂ 11l / min
- µ-wave power 2.5 Kw
- production = 490 g / h of silicon powder, ie an energy yield of 5.15 Kwh / kg of powder and 7.90 KWh of electricity / kg of powder (100% conversion, yield or generator 66%).

On a étiré un monocristal à partir des poudres obtenues ainsi. L'analyse du monocristal a révélé 7 10¹⁷ atome/cm³ d'oxygène et 10 10¹⁷ atome/cm³ de carbone.A single crystal was drawn from the powders thus obtained. Analysis of the single crystal revealed 7 10¹⁷ atom / cm³ of oxygen and 10 10¹⁷ atom / cm³ of carbon.

Exemple 2Example 2

Avec le même réacteur et les débits suivants :
SiH₄      9,5 l/mn
Ar      3 l/mn
N₂      14 l/mn
pour une puissance de 3,125 KW, on a obtenu 665 g/h de poudre de silicium soit un rendement de 4,69 KWh µ-onde/kg poudre et 7,20 KW/h électrique­/kg poudre (conversion 100%)With the same reactor and the following flow rates:
SiH₄ 9.5 l / min
Ar 3 l / min
N₂ 14 l / min
for a power of 3.125 KW, 665 g / h of silicon powder were obtained, ie a yield of 4.69 KWh µ-wave / kg powder and 7.20 KW / h electric / kg powder (100% conversion)

Exemple 3.Example 3.

Avec le même réacteur ( et d₅ = 25 mm)
et les débits suivants :
    SiH₄ : 12 l/mn
    Ar : 2,5l/mn
    N₂ : 12 l/mn
pour un puissance de 3,2 KW, on a obtenu 840 g/h de poudre de silicium, soit un rendement de 3,81 KWh/kg de poudre et 5,86 KWh électrique/kg poudre (conversion 98,3 %).With the same reactor (and d₅ = 25 mm)
and the following debits:
SiH₄: 12 l / min
Ar: 2.5l / min
N₂: 12 l / min
for a power of 3.2 KW, 840 g / h of silicon powder were obtained, ie a yield of 3.81 KWh / kg of powder and 5.86 KWh of electricity / kg of powder (conversion 98.3%).

Les diamètres d₁ à d₆ sont définis sur la figure 1.The diameters d₁ to d₆ are defined in Figure 1.

Claims (15)

1.- Torche à plasma micro-onde, caractérisée en ce qu'elle comporte au moins une conduite d'amenée de gaz (1,2) ; une cavité résonnante (3) formant autour de ladite conduite un manchon ouvert du coté de la sortie de ladite conduite et comportant une ouverture latérale (4) ; une structure coaxiale de transition perpendiculaire au manchon comportant d'une part un tube externe (5) raccordé à l'ouverture latérale (4) du manchon et d'autre part un organe interne (6) dont l'une des extrémités (20) est au contact de ladite conduite et dont l'autre extrémité est au contact de la face externe d'un guide d'onde (8) et porte une pièce de transition (7) disposée dans le guide d'ondes (8) ; ledit guide d'onde (8) d'alimentation en énergie micro-ondes à section rectangulaire et perpendiculaire à la structure coaxiale (5,6) étant pourvu d'une ouverture (27) où est raccordé le tube externe (5) de la dite structure ; des moyens d'alimentation en gaz de gainage dans le guide d'onde (8) et/ou la structure coaxiale (5,6) et/ou le manchon ; éventuellement des moyens d'accord ; et éventuellement des moyens d'allumage du plasma.1.- microwave plasma torch, characterized in that it comprises at least one gas supply pipe (1,2); a resonant cavity (3) forming around said pipe a sleeve open on the side of the outlet of said pipe and having a lateral opening (4); a coaxial transition structure perpendicular to the sleeve comprising on the one hand an external tube (5) connected to the lateral opening (4) of the sleeve and on the other hand an internal member (6) of which one of the ends (20) is in contact with said pipe and the other end of which is in contact with the external face of a waveguide (8) and carries a transition piece (7) disposed in the waveguide (8); said wave energy supply waveguide (8) of rectangular section and perpendicular to the coaxial structure (5,6) being provided with an opening (27) where the external tube (5) of the said structure; cladding gas supply means in the waveguide (8) and / or the coaxial structure (5,6) and / or the sleeve; possibly means of agreement; and possibly plasma ignition means. 2.- Torche à plasma selon la revendication 1, caractérisée en ce que le tube externe (5) est raccordé de façon étanche à l'ouverture latérale (4) et/ou au guide d'onde (8).2.- plasma torch according to claim 1, characterized in that the external tube (5) is tightly connected to the lateral opening (4) and / or to the waveguide (8). 3.- Torche à plasma selon la revendication 1 ou 2, caractérisée en ce que le guide d'onde (8) est relié à une source (21) de gaz de gainage et est muni de part et d'autre de la pièce de transition (7) de moyens d'étanchéité au gaz.3.- plasma torch according to claim 1 or 2, characterized in that the waveguide (8) is connected to a source (21) of cladding gas and is provided on either side of the piece of transition (7) of gas sealing means. 4.- Torche selon l'une des revendications 1 à 3, caractérisée en ce que les moyens d'étanchéité (11,12,13) au gaz sont conducteurs et comportent au moins une fenêtre rectangulaire (11) en matériau transparent aux micro-ondes, deux brides rectangulaires (12,13) enserrant la fenêtre, des moyens d'étanchéité au gaz (14,15) entre la fenêtre et les brides, et des moyens d'étanchéité (16) au gaz entre la bride (13) située en regard de la portion (24) du guide d'onde étanche au gaz et ladite bride.4.- Torch according to one of claims 1 to 3, characterized in that the sealing means (11,12,13) to the gas are conductive and comprise at least one rectangular window (11) made of material transparent to micro- waves, two rectangular flanges (12,13) enclosing the window, gas sealing means (14,15) between the window and the flanges, and gas sealing means (16) between the flange (13) located opposite the portion (24) of the gas-tight waveguide and said flange. 5.- Torche à plasma selon la revendication 1 ou 2, caractérisée en ce que le manchon (3) est relié à une source de gaz de gainage et la structure coaxiale (5,6) est muni de moyens d'étanchéité au gaz.5.- plasma torch according to claim 1 or 2, characterized in that the sleeve (3) is connected to a sheath gas source and the coaxial structure (5,6) is provided with gas sealing means. 6.- Torche selon l'une des revendications 1 à 5, caractérisée en ce que l'extrémité fermée du manchon est une bride annulaire traversée à joint étanche par des moyens de réglage d'un piston annulaire (9), la bride et le piston étant traversés par la conduite d'amenée de gaz (1,2).6. Torch according to one of claims 1 to 5, characterized in that the closed end of the sleeve is an annular flange crossed gasketed by means of adjustment of an annular piston (9), the flange and the piston being traversed by the gas supply pipe (1,2). 7.- Torche selon l'une des revendications 1 à 6, caractérisée en ce que la conduite d'amenée (1,2) de gaz est coaxiale.7.- Torch according to one of claims 1 to 6, characterized in that the gas supply line (1,2) is coaxial. 8.- Torche selon l'une des revendications 1 à 7, caractérisée en ce que les longueurs de la conduite d'amenée de gaz et de la sortie du manchon sont réglables.8.- Torch according to one of claims 1 to 7, characterized in that the lengths of the gas supply pipe and the outlet of the sleeve are adjustable. 9.- Torche selon l'une des revendications 1 à 8, caractérisée en ce que l'extrémité (30,31,32) de la conduite d'amenée de gaz et de la sortie du manchon sont arrondies.9. Torch according to one of claims 1 to 8, characterized in that the end (30,31,32) of the gas supply pipe and the outlet of the sleeve are rounded. 10.- Torche à plasma selon l'une des revendications 1 à 9, caractérisée en ce que la pièce de transition (7) est réglable.10.- plasma torch according to one of claims 1 to 9, characterized in that the transition piece (7) is adjustable. 11.- Torche à plasma selon l'une des revendications 1 à 10, caractérisée en ce que la conduite d'arrivée est coaxiale, la conduite intérieure étant constitué au moins en partie d'un matériau réfractaire.11.- plasma torch according to one of claims 1 to 10, characterized in that the inlet pipe is coaxial, the inner pipe being made at least in part of a refractory material. 12.- Dispositif étanche à plasma micro-onde pour la fabrication de poudre, du type comportant un générateur micro-ondes (41), une torche à plasma micro-ondes (40,43,48), une enceinte réactionnelle (53), des moyens d'alimentation en gaz réactif (46), en gaz plasmagène (47) et un gaz de gainage (42), des moyens de séparation de poudre et des gaz, des moyens de collection des poudres (51), et des moyens d'évacuation des gaz effluents (52), caractérisé en ce que la torche à plasma est réalisée selon l'une des revendications 1 à 10.12.- Waterproof microwave plasma device for the manufacture of powder, of the type comprising a microwave generator (41), a microwave plasma torch (40,43,48), a reaction chamber (53), means for supplying reactive gas (46), plasma gas (47) and a cladding gas (42), means for separating powder and gases, means for collecting powders (51), and means for discharging the effluent gases (52), characterized in that the plasma torch is produced according to one of claims 1 to 10. 13.- Dispositif étanche selon la revendication 12, caractérisé en ce que le rapport de la longueur et du diamètre de l'enceinte réactionnelle est compris entre 1,5 et 6, de préférence 2 et 4.13. A sealed device according to claim 12, characterized in that the ratio of the length and the diameter of the reaction vessel is between 1.5 and 6, preferably 2 and 4. 14.- Procédé de préparation de poudre, caractérisé en ce que l'on utilise un dispositif selon l'une des revendications 1 à 13 et en ce que le gaz réactif est choisi parmi les silanes, l'ammoniac, les hydrures de bore, les halogènes de Tungstène et de Titane, l'oxygène et les organo métalliques gazeux et leurs mélanges.14.- A method for preparing powder, characterized in that a device is used according to one of claims 1 to 13 and in that the reactive gas is chosen from silanes, ammonia, boron hydrides, Tungsten and Titanium halogens, oxygen and gaseous organo-metals and their mixtures. 15.- Procédé de préparation de poudre, selon la revendication 14, caractérisé en ce que la pression d'utilisation est supérieure ou égale à la pression atmosphérique.15.- A method of preparing powder, according to claim 14, characterized in that the operating pressure is greater than or equal to atmospheric pressure.
EP88401405A 1987-06-10 1988-06-09 Microwave plasma torch, device comprising such a torch and production procedure for powder operating them Expired - Lifetime EP0296921B1 (en)

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FR8708096A FR2616614B1 (en) 1987-06-10 1987-06-10 MICROWAVE PLASMA TORCH, DEVICE COMPRISING SUCH A TORCH AND METHOD FOR MANUFACTURING POWDER USING THE SAME

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2773299A1 (en) * 1997-12-29 1999-07-02 Air Liquide Plasma torch with adjustable injector for gas analysis
EP0930810A1 (en) * 1997-12-29 1999-07-21 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Plasma torch with adjustable distributor and gas analysis system using such a torch
US6236012B1 (en) 1997-12-29 2001-05-22 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Plasma torch with an adjustable injector and gas analyzer using such a torch
WO1999052332A1 (en) * 1998-04-02 1999-10-14 Bluem Heinz Juergen Plasma torch with a microwave transmitter
US6388225B1 (en) 1998-04-02 2002-05-14 Bluem Heinz-Juergen Plasma torch with a microwave transmitter
WO2000035256A1 (en) * 1998-12-07 2000-06-15 Robert Bosch Gmbh Device for producing a free cold plasma jet
US6396214B1 (en) 1998-12-07 2002-05-28 Robert Bosch Gmbh Device for producing a free cold plasma jet
CN105898975A (en) * 2016-06-12 2016-08-24 浙江大学 High-power microwave plasma resonant cavity
CN105898975B (en) * 2016-06-12 2018-07-17 浙江大学 A kind of HIGH-POWERED MICROWAVES plasma resonant
CN113196888A (en) * 2018-12-19 2021-07-30 迪热克塔普拉斯股份公司 Apparatus for treating materials with plasma

Also Published As

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FR2616614A1 (en) 1988-12-16
DK310088D0 (en) 1988-06-08
EP0296921B1 (en) 1992-07-29
CA1311277C (en) 1992-12-08
DE3873193D1 (en) 1992-09-03
FR2616614B1 (en) 1989-10-20
JPS63312907A (en) 1988-12-21
US4924061A (en) 1990-05-08
DK310088A (en) 1988-12-11
DE3873193T2 (en) 1993-02-18

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