Apparatus for producing a silicon-based material

Abstract

The present invention relates to an apparatus for producing a silicon-based material from quartz and a reducing agent, the apparatus comprising: - a reaction chamber (1) for generating a gas containing the silicon-based material; - a condensation chamber (2) for solidifying the silicon-based material present in the gas originating from the reaction chamber (1); and - a duct (3) for conveying the gas between the reaction chamber (1) and the condensation chamber (2), characterised in that the condensation chamber (2) further comprises a vibrator for generating vibrations in a side wall (212) of the condensation chamber (2).

Description

[0001] APPARATUS FOR PRODUCING A SILICON-BASED MATERIAL

[0002] FIELD OF THE INVENTION

[0003] The present invention relates to the general technical field of producing a silicon-based material such as silicon(II) monoxide.

[0004] More specifically, the invention relates to the continuous production - as opposed to batch production (or "batch", according to the terminology used in the field of industrial processes) - of a silicon-based material by quartz reduction.

[0005] BACKGROUND OF THE INVENTION

[0006] Silicon(II) monoxide (silicon(II) oxide) is a chemical compound with the formula SiO where silicon is present in a +2 oxidation state. In the vapor phase, silicon(II) monoxide is a diatomic molecule.

[0007] Silicon monoxide (SiO) can be obtained by partial chemical reduction of silicon dioxide (SiO2) in the presence of silicon (Si) according to the following reaction:

[0008] S1O2 + Si 2 SiOf

[0009] To produce silicon monoxide (SiO) using this reaction, a mixture of silicon (Si) and silicon dioxide (SiO2) is heated to a sublimation temperature of silicon(II) monoxide (SiO). When the reaction occurs at atmospheric pressure, the sublimation temperature is 1600°C. When the reaction occurs in a vacuum, the sublimation temperature is significantly lower, around 1200°C.

[0010] Heating the mixture of silicon (Si) and silicon dioxide (SiO2) allows the generation of a gas containing silicon monoxide (SiO) by chemical reduction. This gas is then cooled to a temperature below 800°C. The cooling of the gas containing silicon monoxide (SiO) is carried out quickly to limit the risks of restructuring, by disproportionation, of silicon monoxide (SiO) in the form of silicon (Si) and silicon dioxide (SiO2).

[0011] Rapid cooling of the gas containing silicon monoxide (SiO) induces, by condensation, the formation of an amorphous material, (SiO)n.

[0012] Such a glassy material based on silicon monoxide (SiO) is commercially available and can be used for various applications in the fields of optics or optoelectronics (deposition of a layer of SiO on a support), or in the field of rechargeable lithium-based batteries (manufacture of anodes in particular).

[0013] Various processes for producing silicon monoxide (SiO) from a mixture of silicon (Si) and quartz (SiO2) have already been proposed.

[0014] For example, WO 03 / 025246 describes a method for producing a silicon monoxide material in equipment comprising a reaction chamber and a precipitation chamber located above the reaction chamber. The method comprises the following steps:

[0015] - mixing a silicon powder (Si) and a silicon dioxide powder (SiO2) in the reaction chamber,

[0016] - evacuating and heating the reaction chamber to generate silicon monoxide (SiO) gas, and

[0017] - the precipitation of silicon monoxide (SiO) contained in the gas on a precipitation substrate included in the precipitation chamber, the precipitation chamber having walls inclined at an angle of between 1° and 45°.

[0018] According to WO 03 / 025246, the presence of inclined walls makes it possible to limit the deposition of silicon monoxide (SiO) on them. Document WO 2017 / 004818 describes a method for producing a silicon oxide compound in equipment comprising:

[0019] - a reaction vessel designed to receive a raw material and allow the generation of a gas containing the silicon oxide compound,

[0020] - a heating oven, and

[0021] - a collector located outside the heating furnace, to precipitate the gas containing the silicon oxide compound and form silicon oxide in the solid state.

[0022] According to WO 2017 / 004818, the fact that the collector is offset relative to the heating furnace allows for a faster and more economical production process from the point of view of energy consumption since it is no longer necessary to cool the reaction vessel at each cycle of use of the equipment.

[0023] A disadvantage of these different processes and equipment is that they are configured for the batch production of silicon monoxide. In particular, the equipment according to WO 03 / 025246 and WO 2017 / 004818 must be cleaned after each use. Furthermore, the productivity of these processes and equipment is limited by the fact that the batch processing time is quite long. Indeed, at each new use, it is necessary to carry out: o the loading of the reaction chamber or vessel, and possibly its cleaning, o the evacuation of the reaction chamber or vessel, o the temperature rise of the reaction chamber or vessel, o the cooling and atmospheric pressure of the equipment for the recovery of the solid silicon monoxide material and the solid silicon oxide compound.

[0024] To overcome these drawbacks, document US 7,431,899 proposes an apparatus for the continuous production of silicon monoxide (SiO). The apparatus comprises a system for continuously supplying silicon (Si) and silicon dioxide (SiCh), a reaction chamber for carrying out the chemical reaction of oxidation of silicon (Si) in order to produce the gas containing silicon monoxide (SiO), and a deposition chamber into which the gas from the reaction chamber is transferred, the deposition chamber making it possible, by cooling the gas containing silicon monoxide (SiO), to produce silicon monoxide (SiO) in solid phase depositing on a substrate. To enable continuous production of silicon monoxide, the authors propose the use of a recovery system based on the principle of scraping the substrate to detach the silicon monoxide (SiO) crystals deposited thereon.For this purpose, the deposition chamber includes a mechanical scraper to scrape the substrate.

[0025] A disadvantage of this technique is that mechanical scraping induces contamination of the silicon monoxide (SiO) crystals by the material constituting the scraper, silicon monoxide (SiO) crystals being very abrasive.

[0026] An aim of the present invention is to propose a method for the continuous production of a silicon-based material making it possible to overcome at least one of the aforementioned drawbacks.

[0027] In particular, an aim of the present invention is to provide a method and a device allowing the continuous production of a silicon-based material, such as silicon (Si) and / or silicon monoxide (SiO).

[0028] BRIEF DESCRIPTION OF THE INVENTION

[0029] To this end, the invention provides an apparatus for producing a silicon-based material - such as silicon and / or silicon monoxide - from reactants, said reactants comprising quartz and a reducing agent - such as carbon or metallurgical silicon - wherein the apparatus comprises:

[0030] - a reaction chamber for producing a gas containing the silicon-based material, said reaction chamber comprising: o a housing for carrying out a quartz reduction reaction, o a tank in the housing intended to contain the reactants, o a reactant supply system for introducing the reactants into the tank, o a heating system for heating the reactants contained in the tank,

[0031] - a condensation chamber for solidifying the silicon-based material contained in the gas from the reaction chamber, said condensation chamber including: o a precipitation box defining a space for the solidification of the silicon-based material contained in the gas from the reaction chamber, said precipitation box comprising at least one lateral partition, o a cooling system for cooling the gas from the reaction chamber, said cooling system being in thermal contact with the precipitation box, and o an extraction nozzle for collecting and extracting the solidified silicon-based material, said extraction nozzle being connected to the precipitation box,

[0032] - a conveying pipe for the circulation of the gas containing the silicon-based material between the reaction chamber and the condensation chamber, said conveying pipe being connected to the housing on the one hand, and to the precipitation box on the other hand, remarkable in that the condensation chamber further comprises a vibrator associated with the side partition to induce the generation of vibrations in said side partition.

[0033] As will become clear in the following, the vibrations generated by the vibrator in the side wall facilitate the detachment of the silicon-based material likely to be deposited on the said side wall.

[0034] This improves the efficiency of the apparatus according to the invention by limiting the risk of depositing a thick layer of material on the side partition, such a thick layer reducing the efficiency of the cooling of the gas coming from the reaction chamber, and therefore of the apparatus.

[0035] Preferred but non-limiting aspects of the apparatus according to the invention are as follows:

[0036] - the side partition may comprise a layer of non-stick material such as a ceramic layer, or a layer of metal oxides or a layer of fluoropolymer;

[0037] - the side partition may have the shape of a truncated cone, a generator of the side partition forming a non-zero angle with a vertical axis;

[0038] - the vibrator can be a mechanical vibrator;

[0039] - the mechanical vibrator can be configured to exert a force on the lateral partition along a main axis inclined at a non-zero angle relative to the lateral partition, said non-zero angle being greater than 45° and less than 135°, preferably between 60° and 120°, in particular of the order of 90°;

[0040] - the mechanical vibrator may extend outside the side partition, said mechanical vibrator being mechanically connected to the side partition by a mechanical connecting means, such as a rod in contact on the one hand with the side partition, and on the other hand with the mechanical vibrator;

[0041] - the vibrator can be an acoustic vibrator;

[0042] - the acoustic vibrator may comprise a plurality of transducers arranged on an internal face and / or on an external face of the side partition, said transducers having respective resonance frequencies;

[0043] - the supply system may comprise: o a receiving bowl intended to contain a reserve of reagents, o a distribution channel for the circulation of the reagents between the receiving bowl and the tank, and o at least two valves to authorize or stop the circulation of the reagents between the receiving bowl and the tank;

[0044] - the extraction nozzle may comprise: o a truncated funnel composed of a truncated side wall, a larger diameter upper edge of the truncated side wall being connected to the side partition, and o a tube mounted on a smaller diameter lower edge of the truncated side wall, o at least two valves to allow or prohibit the circulation of the silicon-based material between the truncated funnel and the outside of the condensation chamber;

[0045] - the apparatus may also comprise a suction pump connected to the condensation chamber, to generate a vacuum in the reaction chamber, in the condensation chamber and in the delivery pipe.

[0046] BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Other advantages and characteristics of the apparatus for producing a silicon-based material according to the invention will emerge more clearly from the following description of several variant embodiments, given as non-limiting examples, from the appended drawings in which:

[0048] - Figure 1 is a schematic representation of a first embodiment of an apparatus for producing silicon-based material,

[0049] - Figure 2 is a schematic representation of a second embodiment of the silicon-based material production apparatus.

[0050] DETAILED DESCRIPTION OF THE INVENTION

[0051] Various embodiments of the invention will now be described with reference to the figures. In these various figures, equivalent elements are designated by the same reference numeral. In the following, the invention will be presented with reference to the formation of a silicon monoxide powder from quartz and a reducing agent such as silicon, it being understood that the invention can also be used for the formation of silicon from quartz and carbon-based reducing agents, or for the formation of both silicon and silicon monoxide.

[0052] 1. General information

[0053] With reference to Figure 1, the apparatus according to the invention comprises:

[0054] - a reaction chamber 1,

[0055] - a condensation chamber 2, and

[0056] - a delivery line 3.

[0057] Reaction chamber 1 allows the generation of a gas containing the silicon-based material, in particular silicon monoxide (II).

[0058] The condensation chamber 2 makes it possible to cool the gas containing the silicon-based material in order to form crystals of silicon-based material by condensation of said gas.

[0059] Advantageously, the reaction chamber 1 and the condensation chamber 2 are distinct and separate, said chambers 1, 2 being connected via the conveying pipe 3. This makes it possible in particular to use reaction and condensation chambers 1, 2 of different shapes and dimensions. This also makes it possible to reduce the height of the apparatus.

[0060] The conveying pipe 3 allows the circulation of the gas containing the silicon-based material between the reaction chamber 1 and the condensation chamber 2. To do this: - one 31 of the ends of the conveying pipe 3 is connected to an opening made in the reaction chamber 1, for example at the level of an upper part of the reaction chamber 1,

[0061] - the other 32 of the ends of the conveying pipe 3 is connected to an opening 111 provided in the condensation chamber 2, for example at the level of an upper part of the condensation chamber 2.

[0062] In certain embodiments, the device may further comprise a thermally insulating structure associated with the conveying pipe 3. Such a thermally insulating structure allows:

[0063] - to reduce heat losses during the passage of the gas containing silicon monoxide (II) from the reaction chamber 1 to the condensation chamber 2 and,

[0064] - to limit the parasitic condensation of silicon monoxide on the internal face of the conveying pipe 3 which reduces the material yield of the reaction and can cause blockage of the pipe 3.

[0065] Since such a thermally insulating structure is known to those skilled in the art, it will not be described in more detail below. This thermally insulating structure may, for example, be composed of a thick ceramic lining of aluminum oxide arranged around or inside the conveying pipe 3.

[0066] 2. Reaction chamber

[0067] Reaction chamber 1 allows:

[0068] - on the one hand to contain the reagents - namely quartz and the reducing agent(s) - used for the production of the silicon-based material, and

[0069] - on the other hand, heating said reagents to a high temperature to induce the partial chemical reduction reaction of the quartz in order to obtain the gas containing the silicon-based material. With reference to Figure 1, the reaction chamber 1 comprises:

[0070] - accommodation 11,

[0071] - a 12 reagent supply system,

[0072] - a heating system 13, and

[0073] - a tank 14 intended to contain the reagents.

[0074] 2.7. Accommodation

[0075] The housing 11 makes it possible to confine the gas generated during the partial chemical reduction reaction of quartz. The housing 11 is preferably sealed.

[0076] The housing 11 may be configured to withstand pressures below atmospheric pressure. Indeed, in certain embodiments (as illustrated in FIG. 2), the apparatus may comprise one (or more) suction pump(s) 4 for generating a vacuum (or obtaining an inert atmosphere) in the reaction chamber 1, the condensation chamber 2 and the delivery pipe 3. In other words, the suction pump 4 makes it possible to reduce the pressure inside the reaction chamber 1, the condensation chamber 2 and the delivery pipe 3 to a value below atmospheric pressure. This makes it possible to limit the temperature necessary for initiating the partial chemical reduction reaction of quartz.

[0077] Furthermore, the housing 11 is configured to withstand temperatures greater than or equal to 1000°C, in particular between 1200°C and 1800°C.

[0078] The housing 11 may be cylindrical, or of any other shape known to those skilled in the art. With reference to FIG. 1, the housing 11 comprises a bottom 112, one (or more) side wall(s) 113, and an upper wall 114. In the embodiments illustrated in FIGS. 1 and 2, the upper wall 114 comprises the opening 111 allowing the circulation of the gas containing the silicon-based material between the reaction chamber 1 and the conveying pipe 3. In certain alternative embodiments, the reaction chamber 1 may comprise a thermally insulating structure 115 associated with the housing 11 to reduce heat losses in the housing 11. Such a thermally insulating structure 115 may be composed of a thick ceramic lining of aluminum oxide (alumina or silicon carbide) arranged around the housing 11.

[0079] 2.2. Power supply system

[0080] The reagent supply system 12 makes it possible to fill the tank 14 with quartz and reducing agent(s).

[0081] The power supply system 12 includes:

[0082] - a receiving bowl 121 intended to contain a reserve of quartz and reducing agent(s),

[0083] - a distribution channel 122 for the circulation of quartz and the reducing agent(s), and

[0084] - one (or more) sealed valve(s) 123 to allow or stop the circulation of quartz and the reducing agent(s).

[0085] The receiving bowl 121 comprises a bottom in which a through-hole is provided connected to one end of the distribution channel 122, the other end of the distribution channel 122 opening into the tank 14.

[0086] The valve(s) 123 is (are) mounted on the distribution channel 122.

[0087] When the apparatus is used at atmospheric pressure, the supply system may include a valve 123. A controller (not shown) allows the valve to be controlled from a deactivated state to an activated state (and from an activated state to a deactivated state):

[0088] - the valve blocking the passage of reagents (quartz + reducing agent(s)) between the receiving bowl 121 and the tank 14 in the deactivated state, - the valve authorizing the passage of reagents (quartz + reducing agent(s)) between the receiving bowl 121 and the tank 14 in the activated state.

[0089] When the apparatus is used at a pressure lower than atmospheric pressure (for example under vacuum), the supply system may comprise two valves 123a, 123b, as illustrated in FIG. 2. These first and second valves 123a, 123b define a sealed compartment C between the receiving bowl 121 and the tank 14 (and more generally between the outside and the inside of the housing 11 of the reaction chamber 1). A controller (not shown) makes it possible to control the first and second valves. To fill the compartment C, the controller activates the first valve 123a and deactivates the second valve 123b. The reactants (quartz + reducing agent(s)) flow by gravity from the receiving bowl 121 to the compartment C. When the compartment C is filled with reactants, the controller deactivates the first valve 123a, then activates the second valve 123b. The reagents flow by gravity from compartment C to tank 14.Once the compartment is emptied, the controller deactivates the second valve 123b and a new filling cycle can be initiated (activation of the first valve 123a for filling compartment C, etc.). The presence of two valves 123a, 123b makes it possible to maintain the housing 11 at a pressure lower than atmospheric pressure during the filling of the tank 14.

[0090] 2.3. Heating system

[0091] The heating system 13 allows the reactants to be heated to induce the chemical reduction reaction of quartz.

[0092] The heating system 13 may be of any type known to those skilled in the art. In particular, the heating system 13 may be of the resistive type or of the inductive type or a gas burner. In the embodiment illustrated in FIGS. 1 and 2, the heating system 13 comprises one (or more) MoSi2 (molybdenum disilicate) resistor(s) arranged on the side wall(s) and possibly the bottom of the housing 11.

[0093] Alternatively, the heating system 13 may be of the arc furnace type. The arc furnace makes it possible to heat the reactants at high temperature to induce the chemical reduction reaction of the quartz in order to produce the gas containing the silicon-based material, and in particular silicon (II) monoxide.

[0094] To form an electric arc for heating the reactants, the arc furnace includes electrodes powered either from a direct current source or from an alternating current source.

[0095] Preferably, the electrodes are placed in the axis of the housing 11 so as to be stressed in a relatively symmetrical manner. More precisely, each electrode may consist of a cylindrical graphite bar extending vertically.

[0096] The arc furnace can include:

[0097] - one (or more) mobile electrode(s) held by one (or more) support(s) not shown, the (or each) mobile electrode being able to be introduced into the housing 11 by passing (each) through a through hole made in the upper wall 114,

[0098] - one (or more) fixed electrode(s) housed in the bottom of the tank 14.

[0099] Support(s) holding the movable electrode(s) allow the distance between the ends of the fixed and movable electrode(s) to be varied to control the quantity of energy transferred to the reactants contained in the tank 14.

[0100] As mentioned earlier, each electrode is connected to either a direct current source or an alternating current source. One advantage of a direct current supply is that the electrodes are not subject to the electromagnetic effects that electrodes in a furnace powered by an alternating current source experience.

[0101] In the case of a direct current power supply:

[0102] - the movable electrode(s) can be connected to the positive pole of the direct current source to form an anode,

[0103] - the fixed electrode(s) can be connected to the negative pole of the direct current source and form a cathode.

[0104] Since the arc furnace is of a type known per se to those skilled in the art, its operation will not be described in more detail below.

[0105] 2.4. Tank

[0106] As illustrated in Figures 1 and 2, the tank 14 may consist of a graphite carcass coated externally with a refractory lining. Alternatively, the tank 14 may be made of alumina, silica, metal or silicon carbide (SiC).

[0107] Tank 14 (or crucible) is intended to contain the reagents, but also the by-products resulting from the chemical reduction reaction of quartz.

[0108] With reference to Figure 2, the tank 14 comprises a bottom 141, one (or more) side wall(s) 142, and an upper opening 143. A-A' is a longitudinal central axis of the device which is vertical when the device is placed on a horizontal flat surface. A side wall of the housing 11 is substantially centered on the axis A-A'.

[0109] In the following, the description is oriented by considering that the terms “upper” and “top” correspond to a direction generally parallel to the axis A-A’ and going from the bottom 141 towards the opening 143, while the terms “lower” and “bottom” correspond to an opposite direction. When the heating system 13 comprises an arc furnace, the bottom 141 of the tank 14 may comprise a stud projecting towards the inside of the tank 14. More precisely, the stud projects from the bottom 141 and extends along the axis A-A’ towards the opening 143. The stud may be made of an electrically conductive material and constitute one of the electrodes of the arc furnace (typically the fixed electrode). Alternatively, the bottom 141 may be without a stud and comprise only a circular recess through which one of the electrodes of the arc furnace is mounted.As a further variant, the bottom 141 of the tank 14 may be devoid of a stud and a circular recess, in particular in the case where the electrode (or electrodes) of the arc furnace is (are) mounted above the tank 14.

[0110] The tank 14 also comprises a pouring channel (or channels) (not shown) for discharging the reaction by-products contained in the tank 14 to an external pocket intended to receive it for subsequent storage. A closure system - such as a plug made of carbon material - may be provided for opening and closing the pouring channel (or channels).

[0111] 3. Condensation chamber

[0112] Condensation chamber 2 solidifies the silicon-based material - in particular silicon monoxide (II) - contained in the gas from reaction chamber 1.

[0113] The condensation chamber 2 comprises a precipitation box 21, a cooling system 22, a vibrator 23 and an extraction nozzle 24.

[0114] 3.1. Precipitation box

[0115] The precipitation box 21 may be cylindrical in shape. It comprises, for example, a side partition 212 and possibly an upper partition and / or a lower partition. When the precipitation box 21 comprises an upper partition, the latter comprises a through-orifice connected to the conveying pipe 3 to allow the introduction - into the precipitation chamber 2 - of the gas from the reaction chamber 1. Similarly, when the precipitation box 21 comprises a lower partition, the latter comprises a through-orifice connected to the extraction nozzle 24.

[0116] When the precipitation box 21 is without an upper partition, an upper peripheral edge 211 of the side partition 212 is connected to the conveying pipe 3. When the precipitation box 21 is without a lower partition, a lower peripheral edge 213 of the side partition 212 is connected to the extraction nozzle 24.

[0117] Advantageously, the lateral partition 212 (or all the partitions) of the precipitation box 21 may comprise a layer of smooth non-stick material such as a ceramic layer, or a layer of metal oxides or a fluoropolymer layer. This makes it possible to promote / simplify the detachment of the solidified silicon monoxide deposited on the internal face of the lateral partition 212.

[0118] Furthermore, the lateral partition 212 of the precipitation box 21 may have a truncated cone shape. In particular, the generatrix of the lateral partition 212 may have a non-zero angle (in particular between 1 and 45°) with the vertical axis A-A'. This also makes it possible to promote / simplify the detachment of the solidified silicon monoxide deposited on the internal face of the lateral partition 212.

[0119] 3.2. Cooling system

[0120] The condensation chamber 2 also comprises a cooling system 22 composed for example of one (or more) heat exchanger(s) in which a heat transfer fluid circulates. The integration of a cooling system 22 makes it possible to rapidly cool the gas coming from the reaction chamber 1 in order to solidify the silicon monoxide (II) on the internal face of the side partition 212.

[0121] This rapid cooling of the gas limits the risks of restructuring, by disproportionation, of silicon monoxide (SiO) in the form of silicon (Si) and silicon dioxide (SiO2).

[0122] In the embodiments illustrated in Figures 1 and 2, the cooling system 22 comprises a coil surrounding the side wall 212 over its entire height. A heat transfer fluid - such as water - circulates in the coil.

[0123] This allows the temperature of the gas containing silicon monoxide (II) to be reduced:

[0124] - from a temperature of 1200°C to a temperature below 800°C when the device is used at a pressure below atmospheric pressure, or

[0125] - from a temperature of 1600°C to a temperature below 800°C when the device is used at atmospheric pressure.

[0126] The cooling of the gas induces the solidification of the silicon monoxide contained therein. This solidified silicon monoxide is deposited on the internal face of the lateral partition 212 of the precipitation box 21.

[0127] 3.3. Vibrator

[0128] In order to ensure the efficiency of the gas cooling, the precipitation box 21 also comprises a vibrator 23 configured to generate vibrations on the surface of the side partition 212.

[0129] The generation of vibrations makes it possible to detach the solidified silicon monoxide (II) deposited on the internal face of the lateral partition 212. Thus, the presence of a vibrator 23 makes it possible to limit the thickness of the silicon monoxide layer CM deposited on the internal face of the lateral partition 212 in order to ensure effective cooling of the gas contained in the condensation chamber 2.

[0130] Indeed, the deposition of too thick a layer CM of silicon monoxide on the internal face of the side partition 212 would prevent the efficient transfer of heat between the inside and the outside of the condensation chamber 2, which would prevent the rapid cooling of gases containing the silicon-based material (silicon monoxide).

[0131] The vibrator 23 may be of the acoustic type, that is to say a vibrator converting electrical energy into acoustic energy in the ultrasonic range.

[0132] Alternatively, the vibrator 23 may be of the mechanical type, that is to say a mechanical system generating vibrations using a rotary, linear or electromagnetic mechanism.

[0133] 3.3.1. Acoustic vibrator

[0134] In the case of an acoustic vibrator, it comprises one (or more) transducer(s) and one (or more) generator(s) remote from the transducer(s) to supply the transducer(s) with electrical energy.

[0135] Each transducer is composed of:

[0136] - a ceramic made from a homogeneous or piezocomposite material

[0137] - and possibly an adjustment module (not shown).

[0138] Each transducer constitutes a resonant element, like a tuning fork. The transducer(s) may be arranged on the inner face or (preferably on) the outer face of the lateral partition 212. In the embodiments illustrated in FIGS. 1 and 2, the vibrator 23 comprises a plurality of transducers arranged on the outer face of the lateral partition 212, and more precisely around the cooling system 22.

[0139] According to the invention, each transducer produces in the lateral partition 212, waves with a frequency between 20 kHz and 5 MHz, preferably of the order of 100 kHz. This makes it possible to promote the detachment of the solidified silicon monoxide (II) deposited on the internal face of the lateral partition 212.

[0140] Advantageously, the waves are well distributed in the precipitation box 21 thanks to the fact that the transducers are placed homogeneously on the lateral partition 212. To obtain a homogeneous acoustic field, small transducers, i.e. less than 10 cm and preferably between 2 cm and 5 cm, can be used. This allows optimal paving. The shape of each transducer can, for example, be circular, square or polygonal.

[0141] Preferably, each transducer has its own resonant frequency. The fact that the natural frequencies of the transducers are different prevents standing waves from being established in the precipitation box 21. This has the advantage of improving the acoustic homogeneity in the precipitation box 21.

[0142] As mentioned above, each transducer may also include a tuning module, which may be a power electronics board. In this case, the transducer's piezoelectric ceramic is powered by the power electronics board, providing it with an alternating voltage corresponding to its own vibration mode.

[0143] 3.3.2. Mechanical vibrator In the case of a mechanical vibrator, this may comprise a core (or weight) mounted mobile in linear translation (along said main axis) on two aligned bearings, and moved by the action of a periodic and alternating electromagnetic field.

[0144] Such a mechanical vibrator is configured to exert an axial force (i.e. directed along a main axis (or direction)) on the lateral partition 212, this force being invariable over time.

[0145] Advantageously, the main axis along which the force is exerted may be inclined relative to the lateral partition 212 to be vibrated, by an angle greater than 45° and less than 135°, preferably between 60° and 120°, in particular close to 90°. This makes it possible to promote the detachment of the solidified silicon (II) monoxide deposited on the internal face of the lateral partition 212.

[0146] The mechanical vibrator may be arranged outside the precipitation box 21 and in particular around the cooling system 22 extending opposite the external face of the lateral partition 212. In this case, the mechanical vibrator is connected to the lateral partition 212 by a mechanical connection means, such as one (or more) rod(s) in contact on the one hand with the external face of the lateral partition 212, and on the other hand with the mechanical vibrator.

[0147] The use of an electromagnetic mechanical vibrator makes it possible to offer a vibration generation solution with a very low cost.

[0148] Such mechanical vibrators also have the following advantages:

[0149] - they are compact,

[0150] - they are of low mass,

[0151] - they are robust,

[0152] - they allow continuous operation and they are capable of applying to the precipitation box 21 - via the mechanical connection means, relatively significant forces, for example of the order of a few tens of newtons.

[0153] 3.4. Extraction nozzle

[0154] The extraction nozzle 24 makes it possible to collect and evacuate the silicon monoxide (II) powder detached from the side partition 212 of the precipitation box 21.

[0155] Advantageously, the extraction nozzle 24 can be positioned under the precipitation box 21 to recover the detached silicon monoxide (II) powder falling by gravity.

[0156] The extraction nozzle 24 includes:

[0157] - a truncated funnel 241 composed of a truncated side wall of which: o the upper edge defines a large diameter upper base fixed to the side partition 212 (or to the lower partition if the precipitation box 21 comprises such a lower partition), and o the lower edge defines a smaller diameter lower base, and a tube 242 mounted at the level of the lower base of the funnel 241.

[0158] The extraction nozzle 24 also comprises one (or more) sealed valve(s) 243 to allow or stop the circulation of the solidified silicon monoxide (II) powder between the truncated funnel 241 and the outside of the condensation chamber 2.

[0159] The valve(s) 243 is (are) mounted on the tube 242.

[0160] When the apparatus is used at atmospheric pressure, the extraction nozzle 24 may comprise a single valve 243 as illustrated in FIG. 1. A controller (not shown) makes it possible to control the valve 243 from a deactivated state to an activated state (and from an activated state to a deactivated state): - the valve 243 blocking the passage of the silicon monoxide (II) powder between the funnel 241 and an external container 5 in the deactivated state,

[0161] - the valve allowing the passage of the silicon monoxide powder (II) between the funnel and the external container 5 in the activated state.

[0162] When the apparatus is used at a pressure lower than atmospheric pressure (for example under vacuum), the extraction nozzle 24 may comprise two valves 243a, 243b, as illustrated in FIG. 2. These first and second valves 243a, 243b define a sealed compartment CE between the funnel 241 and the external container 5 (and more generally between the exterior and the interior of the condensation chamber 2).

[0163] A controller (not shown) is used to control the first and second valves 243a, 243b. To fill the compartment CE, the controller activates the first valve 243a and deactivates the second valve 243b. The silicon monoxide (II) powder flows by gravity from the funnel 241 to the compartment CE. When the compartment CE is filled with powder, the controller deactivates the first valve 243a and then activates the second valve 243b. The powder flows by gravity from the compartment CE to the external container 5. Once the compartment CE is emptied, the controller deactivates the second valve 243b and a new filling cycle can be initiated (activation of the first valve 243a for filling the compartment CE, etc.). The presence of two valves 243a, 243b makes it possible to maintain the precipitation box 21 at a pressure lower than atmospheric pressure during the filling of the external container 5.

[0164] 4. Conclusions

[0165] The device described above allows the continuous production of a silicon-based material:

[0166] - such as silicon monoxide (II) powder, or

[0167] - silicon, or

[0168] - silicon and silicon monoxide, or

[0169] - an intermediate oxide, SiOx (0 <x<2). L’intégration d’un vibrateur permet de décrocher le monoxyde de silicium (II) se solidifiant sur les parois du caisson de précipitation de la chambre de condensation. Ceci limite les risques de dismutation du monoxyde de silicium en garantissant un refroidissement rapide et efficace du gaz généré dans la chambre réactionnelle.

[0170] The reader will understand that numerous modifications can be made to the invention described above without materially departing from the new teachings and advantages described herein.

Claims

CLAIMS 1. Apparatus for producing a silicon-based material - such as silicon or silicon(II) monoxide - from reactants, said reactants comprising quartz and a reducing agent - such as carbon or metallurgical silicon - wherein the apparatus comprises: - a reaction chamber (1) for producing a gas containing the silicon-based material, said reaction chamber comprising: o a housing (11) for carrying out a quartz reduction reaction, o a tank (14) in the housing (11) intended to contain the reactants, o a reagent supply system (12) for introducing the reactants into the tank (14), o a heating system (13) for heating the reactants contained in the tank (14), - a condensation chamber (2) for solidifying the silicon-based material contained in the gas from the reaction chamber (1), said condensation chamber (2) including: o a precipitation box (21) defining a space for the solidification of the silicon-based material contained in the gas from the reaction chamber (1), said precipitation box (21) comprising at least one lateral partition (212), o a cooling system (22) for cooling the gas from the reaction chamber (1), said cooling system being in thermal contact with the precipitation box (21), and o an extraction nozzle (24) for collecting and extracting the solidified silicon-based material, said extraction nozzle being connected to the precipitation box (21), - a conveying pipe (3) for the circulation of the gas containing the silicon-based material between the reaction chamber (1) and the condensation (2), said conveying pipe (3) being connected to the housing (11) on the one hand, and to the precipitation box (21) on the other hand, characterized in that the condensation chamber (2) further comprises a vibrator (23) associated with the side partition (212) to induce the generation of vibrations in said side partition (212).

2. Apparatus according to claim 1, wherein the side wall (212) comprises a layer of non-stick material such as a ceramic layer, or a layer of metal oxides or a layer of fluoropolymer.

3. Apparatus according to any one of claims 1 or 2, in which the lateral partition (212) has a truncated cone shape, a generatrix of the lateral partition (212) forming a non-zero angle with a vertical axis (A-A').

4. Apparatus according to any one of claims 1 to 3, wherein the vibrator (23) is a mechanical vibrator.

5. Apparatus according to claim 4, wherein the mechanical vibrator is configured to exert a force on the lateral partition (212) along a main axis inclined at a non-zero angle relative to the lateral partition (212), said non-zero angle being greater than 45° and less than 135°, preferably between 60° and 120°, in particular of the order of 90°.

6. Apparatus according to any one of claims 4 or 5, wherein the mechanical vibrator extends outside the side partition (212), said mechanical vibrator being mechanically connected to the side partition (212) by a mechanical connecting means, such as a rod in contact on the one hand with the side partition (212), and on the other hand with the mechanical vibrator.

7. Apparatus according to any one of claims 1 to 3, wherein the vibrator (23) is an acoustic vibrator.

8. Apparatus according to claim 7, wherein the acoustic vibrator comprises a plurality of transducers arranged on an inner face and / or on an outer face of the side partition (212), said transducers having respective resonant frequencies.

9. Apparatus according to any one of claims 1 to 8, wherein the power supply system (12) comprises: - a receiving bowl (121) intended to contain a reserve of reagents, - a distribution channel (122) for the circulation of reagents between the receiving bowl (121) and the tank (14), and - at least two valves (123a, 123b) to allow or stop the circulation of reagents between the receiving bowl (121) and the tank (14).

10. Apparatus according to any one of claims 1 to 9, wherein the extraction nozzle (24) comprises: - a truncated funnel (241) composed of a truncated side wall, an upper edge of larger diameter of the truncated side wall being connected to the side partition (212), and a tube (242) mounted on a lower edge of smaller diameter of the truncated side wall, - at least two valves (243a, 243b) to allow or prevent the circulation of the silicon-based material between the truncated funnel (241) and the exterior of the condensation chamber (2).

11. Apparatus according to any one of claims 1 to 10, which further comprises a suction pump (4) connected to the condensation chamber, for generating a vacuum in the reaction chamber (1), in the condensation chamber and in the delivery line (3).

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