• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Process and device for removing the oxides present on the surface of nodules from a metal powder before using it in an industrial process for assembling powder by solid or liquid route, characterized in that it consists in etching said metal powder by contacting it with steam of a solid etching material, and / or by sublimation of a solid etching material followed by a chemical transformation for said metal powder.
    公开号:FR3038623A1
    申请号:FR1556635
    申请日:2015-07-10
    公开日:2017-01-13
    发明作者:Thierry Mazet
    申请人:FIVES；
    IPC主号:
    专利说明:

    METHOD FOR REMOVING OXIDES PRESENT AT THE SURFACE OF NODULES OF A METALLIC POWDER BEFORE USING IT IN AN INDUSTRIAL PROCESS
    The present invention relates to a method and a device for removing the oxide layer covering the nodules of a metal powder, or oxide spots present on the surface of said nodules. It is implemented prior to the use of the metal powder in an industrial process for solid powder assembly, such as sintering, or in liquid form, such as additive powder-melting production, for which the The presence of oxides on the surface of nodules is an obstacle to the smooth running of the industrial process and can degrade the quality of the part. It is particularly applicable to metal powders of oxygen-hungry metals, such as aluminum, titanium, zirconium, chromium, niobium, tantalum, molybdenum and their alloys and more generally those of which does not go through the liquid route.
    The metal powder may be composed of nodules all having the same composition, or a mixture of nodules having at least two different compositions. For example, it may be an aluminum nodule powder or a mixture of aluminum nodules and nickel nodules.
    Some metals, such as aluminum, are very hungry for oxygen. In the open air, their surface is instantly covered with a film of oxides which during assembly operations, requiring the adhesion of nodules to each other or their fusion, affects the quality of the connection. The said layer can then be sufficiently resistant to maintain in its gangue of oxide the liquid phase formed during these operations. The development of the metal powder can be carried out under a partial vacuum or under an inert atmosphere, so as to avoid and / or limit the presence of oxidizing species in the vicinity of the material, in particular when it is heated to a high temperature. However, it is in practice almost impossible to keep this metal powder in a state of non-oxidation, especially when the industrial process using said powder is practiced under air. Thus, the metal powder of these metals is generally oxidized during its use.
    The present invention makes it possible to overcome this problem by making it possible to remove the layer of oxides covering the nodules with a metal powder, or the oxides spots present on the surface of said nodules, at the moment of their use in an industrial process, allowing thus to obtain parts having high mechanical characteristics and / or reinforced properties and free of traces of oxides. The invention consists in particular in a process for removing the oxides present on the surface of nodules from a metal powder before or during the use thereof in an industrial process for assembling metal powder by solid or liquid route , characterized in that it consists in etching said metal powder by putting it in contact with the vapor obtained by sublimation of a solid material stripper and / or by sublimation of a solid material stripper followed by a chemical transformation . In the art, the solid stripping material is generally referred to as "flux".
    The solid stripping material, or flux, is heated to sublimate, it can then undergo a chemical transformation, for example the decomposition of the original molecule of the flux into other distinct molecules. In what follows, the product resulting from the sublimation of the solid-etching material and / or the product resulting from the sublimation of the solid-etching material followed by an "etching solid-solid material" or "steam of solid etching material" will be denoted chemical transformation.
    According to an exemplary embodiment of the invention, the solid etching material is a halide, for example NH 4 F. At atmospheric pressure, it is brought to a temperature of about 200 ° C to obtain its sublimation. The chemical transformation of NH4F can for example lead to the formation of AIF and AIF3. According to another embodiment of the invention, the solid stripping material is K3AIF6-KAIF4 heated to a temperature of about 400 ° C at atmospheric pressure to obtain its sublimation. These two examples of solid materials strippers or flux are particularly suitable for pickling aluminum. The sublimation temperature is reduced when the enclosure in which the flow is placed is placed under a pressure below atmospheric pressure.
    Advantageously, the steam obtained by sublimation of a solid etching material and / or by sublimation of a solid etching material followed by a chemical conversion is entrained by a carrier gas, for example argon. The use of a carrier gas makes it possible to have a total flow rate of carrier gas plus vapor of solid material, which is greater and therefore easier to regulate in flow and pressure.
    According to an exemplary embodiment of the invention, the carrier gas flowing between the nodules of the metal powder and said metal powder constitute a fluidized bed. The invention also consists of a device for implementing the method described above.
    This device comprises a container in which is placed the solid stripping material, a means providing the calories for sublimating the solid stripping material, and a means for contact between the vapor of solid stripping material and the metal powder.
    The means allowing the contact between the vapor of solid stripping material and the metal powder can simply be based on the proximity of the nodules of solid material stripping with the nodules of the metal powder.
    The means allowing the contact between the steam of etching solid material and the metal powder may also be a hopper on which the metal powder rests, said hopper being traversed by steam of etching solid material.
    The means allowing the contact between the vapor of solid stripping material and the metal powder may be the fall of a rain of metal powder in a rising stream of steam of solid stripping material.
    According to an exemplary embodiment of the invention, the device according to the invention comprises a first container in which is placed the solid stripping material, means for sublimating said stripping solid material, a device conducting the vapor of solid stripping material to a second container in which is placed the metal powder. Said containers may constitute a single container having at least two compartments, a first compartment where the solid stripping material is located and a second compartment where the metal powder is located.
    According to one embodiment, the device comprises means for obtaining a fluidized bed in the container where the metal powder is located by the flow of the steam of solid material stripping between the nodules of the metal powder.
    The device comprises means for collecting the gases at the outlet of the container where the metal powder is etched to ensure confinement and / or treatment to neutralize the polluting components of said gases. The invention also consists of an additive manufacturing machine comprising a device as described above for carrying out the method according to the invention.
    The features and advantages of the invention will appear on reading the description which follows, given solely by way of example, and not by way of limitation, with reference to the following appended figures: FIG. 1: schematic representation of a first example of device according to the invention, - Figure 2: schematic representation of a second example of device according to the invention, and - Figure 3: schematic representation of a third example of the device according to the invention.
    To simplify the description, we will consider below that the metal powder to be prepared for use in an industrial process consists of nodules having the same composition. Nevertheless, the invention also applies to metal powder having nodules of different composition and / or dimensions.
    It can be seen in FIG. 1, a first embodiment of the invention. A mixture consisting of nodules 1 of a metal powder 2 to be prepared for use in an industrial process and of nodules 3 of solid etching material 4 for said metal powder is placed on a hopper 5 located in a container 6. The proportion between the nodules 1 of the metal powder 2 and the nodules 3 of the solid etching material 4 is determined according to the nature of the metal powder and of the solid stripping material, the amount of oxides present on the surface of the nodules 1 of the metal powder. 2 and conditions of implementation of the method according to the invention.
    The mixture between the nodules 1 of the metal powder 2 and the nodules 3 of the solid etching material 4 is made in such a way that the nodules 3 of solid etching material 4 are dispersed in the metal powder 2. The quantity of solid etching material 4 is determined according to the size of the nodules 1 of metal powder and according to the ease with which the nodules 3 of solid stripping material will go into the vapor phase during the implementation of the method according to the invention. It is important for the vapor of solid etching material 4 to come into contact with the entire surface of each of the nodules 1 of metal powder 2.
    A carrier gas 7, for example argon, is injected under the hopper 5 via a supply duct 8 comprising a member 9 for isolating and regulating the flow of carrier gas.
    A means 10 makes it possible to bring the mixture composed of nodules 1 of metal powder 2 and nodules 3 of solid stripping material 4 to the temperature required for the process according to the invention. It makes it possible to provide the calories making it possible to bring the solid pickling material to the temperature required to obtain its gasification and then to carry the vapors of solid etching material 4 obtained at the desired temperature to interact with the metal powder 2. This means 10 can for example, be placed on the outer walls of the container 6, and / or inside the container 6 under the hopper 5, and / or on the supply duct. The means 10 can also be a combination of means placed in different places. It may for example be one or more electrical resistors. The container 6 and the supply duct 8 are thermally insulated to prevent heat loss and avoid any risk of burns for operators. Advantageously, the carrier gas 7 is heated before it comes into contact with the mixture of nodules 1 of metal powder 2 and the nodules 3 of solid stripping material 4.
    The flow rate and the feed pressure of the carrier gas 7 are adjusted according to the quantity and the height of the mixture of solid material pickling 4 and metal powder 2 to be treated so as to ensure the levitation of the metal powder.
    The hopper 5 has characteristics which allow the gas flow through its thickness, while maintaining the solid stripping material 4 and the metal powder 2 on the top of its upper face. Its pressure drop makes it possible to ensure a good distribution of the flow of the carrier gas 7 over its entire lower face.
    By circulating around the nodules 3 of solid stripping material 4, the carrier gas 7 facilitates the transport of the solid stripping material 4 through the metal phase. This passes directly from the solid state to the gaseous state, without passing through an intermediate liquid state. The solid stripping material 4 is thus sublimated.
    The intimate contact between the gaseous mixture and the metal powder 2 makes it possible to strip the surface of the metallic nodules 1 by removing all traces of oxides present on the surface of said nodules 1. These oxides are decomposed into gases entrained by the carrier gas and the balance of solid material vapor remover sublimated.
    In the upper part of the container 6, there is a conduit 11, equipped with an isolation member 12, through which escape the gas mixture consisting of the carrier gas 7, the products of the reaction between the vapors from the sublimation of the solid stripping material and the oxides present on the surface of the nodules 1, as well as vapors from sublimation solid material stripper surplus unreacted with the metal oxides. The conduit 11 is connected to a means for collecting and cooling these gases, not shown in FIG. 1. A means for treating the gases collected at the outlet of the container 6 may be located downstream of the conduit 11 so as to directly reject these gases after depollution. This gas treatment means can be deported. In this case, the gases collected at the outlet of the container 6 are encapsulated for their subsequent treatment.
    Advantageously, the flow of the carrier gas 7 between the nodules 1 and 3 leads to the formation of a fluidized bed.
    The inner walls of the container 6 and the hopper 5 are made of or covered with a material compatible with the solid etching material 4 and / or gaseous, and with the temperature level at which these equipments are worn when carrying out the process according to the invention. the invention.
    Once the operation is complete, the assembly is cooled and the container 6 is isolated by means of the members 9 and 12. This container 6 can be used later for feeding the machine which will exploit the metal powder 2 in a industrial process. According to a variant, the container 6 is then placed in an enclosure under a non-oxidizing atmosphere in which a transfer of the metal powder is carried out to a container which will be sealed after filling and subsequently used for feeding the machine that will exploit the metal powder in an industrial process.
    Obviously, since the metal powder 2 is very hungry for oxygen, it is imperative that it be maintained under a non-oxidizing atmosphere between the end of the process according to the invention and its use for an industrial process for which the surface of the nodules 1 of metal powder 2 must be free of oxides.
    The mixture between the etching solid material 4 and the metal powder 2 can be produced just before the deposition thereof on the hopper 5 of the device according to the invention. It can also be performed upstream, the mixture is prepared in the workshop and delivered ready for use. For example, powder of etching solid material 4 and metal powder 2 may be mixed before the assembly is ground in a high energy or planetary mill or in an attritor mill, so as to obtain an intimate mixture. between the two components.
    According to an alternative embodiment, the solid etching material 4 is not in the form of a nodule but covers the surface of the nodules 1 of the metal powder 2. In this case, only the metal powder 2 previously coated with solid material stripper 4 is placed on the hopper 5 of the device according to the invention.
    As an alternative embodiment of the invention, the etching solid material 4 is not mixed with the metal powder 2. The etching solid material 4 is first deposited in the hopper 5 and separated from the metal powder 2 by a screen allowing the passage of the carrier gas and the vapors obtained by sublimation of the solid stripping material without allowing the metal powder 2 to come into contact with the nodules 3 of solid stripping material 4.
    According to another variant embodiment of the invention, no carrier gas 7 is used. In this case, the solid stripping material 4 and the metal powder lie at the bottom of the container 6, the hopper 5 being no longer necessary. In this case, the vapor obtained by sublimation of the etching solid material 4 naturally goes back through the metal powder 2.
    It can be seen in FIG. 2, a second embodiment of the invention. Stripping solid material 4 is placed above a hopper 20 in the lower part 21 of a container 6. The solid stripping material 4 takes for example the form of a powder or pieces of larger dimensions. The container 6 is supplied at its lower part with a carrier gas 7, for example argon. The hopper 20 supports the solid stripping material 4 and the distribution of the carrier gas 7 over the entire section of the container 6.
    In the upper part 22 of the container 6, metal powder 2 is placed above a second hopper 23. A means 24 ensures the mechanical connection between the two parts 21 and 22 of the container 6 and the seal of it.
    A heating means 10 makes it possible to provide the necessary calories to bring the solid etching material 4 to the temperature required to obtain its gasification and then to carry the vapors obtained by sublimation of the solid stripping material to the desired temperature to interact with the metal powder.
    After passing through the first hopper 20, the carrier gas 7 mixes with the steam obtained by sublimation of the solid stripping material 4. The gaseous mixture thus constituted of a portion of carrier gas 7 and a portion of solid material stripper 4 sublimated then passes through the second hopper 23 on which is placed the metal powder 2. Advantageously, the circulation of this gas mixture between the nodules 1 of the metal powder 2 forms a fluidized bed.
    The two hoppers 20 and 23 are such as to allow the gas flow through their thickness, while maintaining the solid material stripper 4 for the hopper 20 and the metal powder 2 for the hopper 23. Their pressure drop allows for ensure a good distribution of the gas flow over their entire section.
    The carrier gas 7 is supplied at a pressure sufficient to flow between the inlet and the outlet of the container 6 despite the loss of load resulting from the hoppers 20 and 23, the solid stripping material 4 and the metal powder 2. A regulating member 9 makes it possible to regulate the flow of carrier gas 7.
    In the upper part of the container 6, there is an outlet 11 through which the gaseous mixture consisting of the carrier gas 7, products of the reaction between the sublimed solid etching material and the oxides present on the surface of the nodules 1, as well as Sublimated excess solid remover material that has not reacted with the metal oxides.
    According to an alternative embodiment of the invention, no carrier gas 7 is used. In this case, the solid pickling material 4 rests at the bottom of the container 6, the hopper 20 being no longer necessary. Only the steam obtained by sublimation of the solid stripping material naturally passes through the hopper 23 on which the metal powder 2 rests.
    It can be seen in FIG. 3, a third embodiment of the invention. The metal powder 2 is discharged continuously by an injector 30 on a hopper 31 placed in the upper part of a container 37. Unlike the hoppers 5, 20, 23 described in the preceding examples of embodiment, the hopper 31 makes it possible to pass from metal powder 2. This hopper 31 behaves a bit like a shower head. The metal powder falls from the hopper 31 in the form of a shower of nodules 1 and is deposited on the bottom of the container 6. In the lower part of the container 6, there is at least one injection point 33 of a mixture 34 of vapors obtained by sublimation of solid etching material and a carrier gas 7. This mixture 34 flows into the container 37 substantially from bottom to top before exiting through an orifice 11 placed in the upper part of the container 37. The nodules 1 are thus placed in a gaseous stream comprising the stream vapor 4, which removes the oxides present on the surface of the nodules 1 of the metal powder 2. The height of the container 37 and the flow rate of the mixture 34 in said containing 37 are determined so that the duration of the fall of a metal nodule 1 in the container 37 is sufficient for the vapors obtained by sublimation of the solid stripping material 4 to remove any trace of oxy from the surface of said nodule. The mixture 34 comes from a container 37 in which pickling solid material 4, placed on a hopper 38 crossed by a flow of carrier gas 7, is sublimated by the calorie intake of a heating means 10.
    In the embodiments of the invention described above, the atmosphere present in the device is advantageously rendered non-oxidizing before the beginning of the implementation of the method according to the invention, for example by placing under partial vacuum or by a sweep of sufficient duration by an inert gas or by common action.
    The process according to the invention can also be directly implemented in the machine in which the industrial process using the metal powder 2 is carried out.
    For example, the method according to the invention can advantageously be implemented in an additive manufacturing machine. Said machine can be supplied with sealed containers containing the previously activated powder according to the invention. It may also contain a device 50 according to the invention to perform in-situ the activation of the powder according to the method of the invention.
    Numerous developments have been made in recent years for the additive manufacturing of 3-dimensional parts from a metal powder, or a mixture of metal powders. This method of manufacture consists of melting successive layers of powder above those previously added, fused and solidified. According to alternative embodiments, the powder is either deposited in the form of a layer above a bed of powder containing the first layers of the already fused and solidified part before being melted, for example according to the melting methods. selective laser or electron beam, or already melted when it is deposited on the substrate, for example by direct laser or electron beam manufacturing method. In this case, the metal powder is injected into a nozzle to form a homogeneous jet, which for example passes through a laser beam which will melt the powder before it is deposited on the substrate.
    However, the additive manufacturing of parts made of materials that are very hungry for oxygen, such as aluminum and some of these alloys that are lightly loaded with alloying elements, is very difficult because of the oxide layer that covers the surface of the alloys. nodules of the metal powder. The invention overcomes this problem by allowing the use of metal powders not covered with oxide layer.
    For an additive manufacturing machine, the metal powder can be treated according to the invention, either before the deposition of the first layer of powder on the work plate, or during and / or after the deposition of each layer of powder. In the case where the pickling of the metal powder is carried out during and / or after the deposition of each layer of powder, the plate on which the piece is made constitutes the hopper 5, 23 according to the embodiments of the invention shown in FIG. Fig. 1 and FIG. 2. Performing this operation during or after the deposition of the metal powder layer requires that the sweeping of the gas flow does not cause excessive displacement of powder on the surface of the deposited layer that is likely to affect the smoothness of the surface and the thickness of the layer. To avoid this difficulty, it may be advantageous to bring the metal powder 2 into contact with the flow vapor 4 before the deposition of the layer.
    This stripping operation of the metal powder can be carried out in a single operation for all of the metal powder necessary for the production of a part, in portions of the total quantity of powder treated successively one after the other, or in portions of the total amount of powder treated continuously. In the latter two cases, the scanning of the metal powder by the gas flow is carried out in a metal powder container of restricted volume placed closer to the working zone and downstream of a larger metal powder container. in the direction of flow of the metal powder. Treatment in this container of a small volume can facilitate the scanning of the metal powder by the sublimed etching solid material.
    According to an illustrative embodiment of the invention according to FIG. 2, for the treatment of aluminum metal powder 2 AI3003. The inner surface of the container 21 is coated with aluminum and the hoppers 20 and 23 are made of aluminum alloy. The carrier gas 7 is argon, the stream 4 is NH4F. The argon is brought to a temperature of 200 ° C. upstream of the hopper 20. The solid stripping material is also brought to a temperature of 200 ° C. to obtain its sublimation. Sublimated pickling solid material then reacts with the walls of the hopper to form AIF and AIF3, the latter being the most stable.
    The sublimed solid etching material reacts with the aluminum oxides AI2O3, located on the surface of the metallic nodules according to the reaction 2NH4F → N2 + 4H2 + F2; 3F2 + Al203 -> / 402 + 2AIF3.
    The metal powder is also maintained at a temperature of about 200 ° C. This relatively low temperature makes it possible to avoid any risk that the aluminum nodules freed of their alumina layer will stick together.
    The gaseous effluents collected at the outlet 26 of the enclosure 6 are treated with lime to neutralize the fluorides.
    权利要求:
    Claims (12)
    [1" id="c-fr-0001]
    A method for removing oxides from the surface of nodules (1) of a metal powder (2) prior to use thereof in an industrial process for assembling metal powder by solid or liquid means, characterized in that it consists of pickling said metal powder by putting it in contact with the steam obtained by sublimation of a solid stripping material and / or by sublimation of a solid stripping material followed by a chemical transformation.
    [2" id="c-fr-0002]
    2. Method according to claim 1, characterized in that the solid stripping material (4) is NH4F and in that it is heated to a temperature of about 200 ° C to obtain its sublimation.
    [3" id="c-fr-0003]
    3. Method according to claim 1, characterized in that the one of a stripping solid material (4) is K3AIF6-KAIF4 and in that it is heated to a temperature of about 400 ° C to obtain its sublimation.
    [4" id="c-fr-0004]
    4. Method according to any one of claims 1 to 3, characterized in that the vapor obtained by sublimation of a solid etching material and / or by sublimation of a solid etching material followed by a chemical transformation is driven by a carrier gas (7).
    [5" id="c-fr-0005]
    5. Method according to any one of claims 1 to 4, characterized in that the carrier gas (7) flowing between the nodules (1) of the metal powder (2) and said metal powder (2) constitute a fluidized bed.
    [6" id="c-fr-0006]
    6. Device (50) for implementing the method described in the preceding claims on a metal powder (2), characterized in that it comprises a container (6, 37) in which is placed the solid stripping material (4) , means (10) providing the calories for subliming the solid stripping material (4), and means (40) for contacting the vapor obtained by sublimation of a solid stripping material and / or by sublimation of a material solid stripper followed by a chemical transformation (4) and the metal powder (2).
    [7" id="c-fr-0007]
    7. Device according to claim 6, characterized in that the means (40) allowing the contact between the steam obtained by sublimation of a solid stripping material and / or by sublimation of a solid stripping material followed by a chemical transformation and the metal powder (2) results from the intimate bond between the nodules (3) of solid stripping material (4) with the nodules (1) of the metal powder (2).
    [8" id="c-fr-0008]
    8. Device according to claim 6, characterized in that the means (40) for contact between the vapor obtained by sublimation of a solid stripping material and / or by sublimation of a solid stripping material followed by a chemical transformation and the metal powder (2) is a hopper (23) on which the metal powder (2) rests, said hopper (23) being traversed by said vapor.
    [9" id="c-fr-0009]
    9. Device according to claim 6, characterized in that the means (40) for contact between the steam obtained by sublimation of a solid stripping material and / or by sublimation of a stripping solid material followed by a chemical transformation ( 4) and the metal powder (2) is the falling of a rain of metal powder (2) in a rising stream of said vapor.
    [10" id="c-fr-0010]
    10. Device according to any one of claims 6 to 9, characterized in that it comprises means (45) for obtaining a fluidized bed in the container (6) by the flow of the vapor obtained by sublimation d a solid material etching and / or sublimation of a solid stripping material followed by a chemical transformation between the nodules (1) of the metal powder (2).
    [11" id="c-fr-0011]
    11. Device according to any one of claims 6 to 10, characterized in that it comprises means for collecting the gas outlet of the container (6) to ensure containment and / or treatment to neutralize their components pollutants of said gases.
    [12" id="c-fr-0012]
    12. Additive manufacturing machine characterized in that it comprises a device according to any one of claims 6 to 11.
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    同族专利:
    公开号 | 公开日
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    EP3320129A1|2018-05-16|
    CN108138335B|2021-06-15|
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    KR20180052602A|2018-05-18|
    US20180221946A1|2018-08-09|
    FR3038623B1|2017-06-30|
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    优先权:
    申请号 | 申请日 | 专利标题
    FR1556635A|FR3038623B1|2015-07-10|2015-07-10|PROCESS FOR REMOVING OXIDES PRESENT AT THE SURFACE OF NODULES OF A METAL POWDER BEFORE USING THE SAME IN AN INDUSTRIAL PROCESS|FR1556635A| FR3038623B1|2015-07-10|2015-07-10|PROCESS FOR REMOVING OXIDES PRESENT AT THE SURFACE OF NODULES OF A METAL POWDER BEFORE USING THE SAME IN AN INDUSTRIAL PROCESS|
    CN201680043709.7A| CN108138335B|2015-07-10|2016-07-08|Method for removing oxides present on the surface of nodules of metal powder before using it in an industrial process|
    KR1020187003724A| KR20180052602A|2015-07-10|2016-07-08|A method capable of removing oxides present on the surface of a nodule of a metal powder before using the metal powder in an industrial method|
    US15/743,325| US11219948B2|2015-07-10|2016-07-08|Method allowing the removal of oxides present on the surface of nodules of a metal powder before using same in an industrial method|
    JP2018520651A| JP2018523018A|2015-07-10|2016-07-08|Method for removing oxides present on nodule surfaces of metal powders before use in industrial processes|
    PCT/EP2016/066363| WO2017009264A1|2015-07-10|2016-07-08|Method allowing the removal of oxides present on the surface of nodules of a metal powder before using same in an industrial method|
    EP16741893.8A| EP3320129A1|2015-07-10|2016-07-08|Method allowing the removal of oxides present on the surface of nodules of a metal powder before using same in an industrial method|
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