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Definitions

• the invention relates to the production of high temperature resistant material in an oxidizing medium, especially in the presence of air, water vapor and, more generally, in the presence of any gaseous or liquid phase containing oxygen or one of its compounds. .
• the invention relates in particular to the production of a piece of refractory material capable of constituting a resistant protection in an oxidizing medium at high temperature.
• the invention also relates to the high-temperature protection in an oxidizing medium of thermostructural composite materials comprising at least part of carbon, the fibers constituting the fibrous reinforcement of these materials being most of the time carbon fibers, the densification matrix of these fibers. materials which may be partly or wholly of carbon, or of a material other than carbon.
• the invention relates more particularly, but not exclusively, to carbon / carbon (C / C) thermostructural composite materials which consist of a carbon fiber reinforcement densified by a carbon matrix.
• thermostructural composite materials are characterized by their mechanical properties which make them suitable for constituting structural parts and by their capacity to retain these mechanical properties at high temperatures.
• the composite materials when they contain carbon, the composite materials have the important disadvantage of oxidizing at 400 ° C in air or in an oxidizing medium and losing some of their thermostructural properties.
• SiC + (barium boron aluminosilicate
• SiC + magnesium boron aluminosilicate
• thermostructural composite materials for example, C / C
• HfB 2 hafnium diboride
• ZrB 2 zirconium diboride
• ZrB 2 and HfB 2 form, under an oxidizing atmosphere, a porous refractory oxide at a temperature above 2000 ° C and a liquid phase B2O3 (melting temperature of about 450 ° C).
• this last liquid phase B2O3 evaporates almost completely when the temperature is above 1800 ° C.
• HfB 2 and ZrB 2 By adding SiC to HfB 2 and ZrB 2 , the oxidation of these compounds leads to a porous refractory skeleton Hf0 2 or Zr0 2 (temperature resistant) coated on the surface by a viscous liquid phase consisting of SiO 2 which has the property to decrease the amount of oxygen diffusing through the oxide layer, and therefore to reduce the rate of oxidation of the protective material.
• the melting temperature of the silica is around 1700 ° C and the boiling temperature is 2700 ° C. At temperatures above 2000 ° C, the silica is in liquid form. Numerous studies have shown that the formation of the initial Si0 2 layer is very fast (quasi-instantaneous nucleation). In addition, the oxidation reaction results in a significant increase in the volume of the material associated with the molar volume variation of one mole of SiO 2 with respect to one mole of SiC. Moreover, its coefficient of thermal expansion is low, allowing a good thermal compatibility with the other layers of refractory oxides present having a thermal expansion coefficient often much higher than that of the composite material. This significant increase in volume and the low permeability of oxygen in silica explain the protective nature of SiO 2 , which is an effective barrier to oxygen diffusion. This is a special case of passive oxidation.
• the object of the invention is to provide a refractory material resistant to high temperature, in particular to oxidation at temperatures greater than or equal to 2000 ° C., under pressure conditions ranging from very low pressure (> 1 Pa) up to at higher values (> 30 MPa).
• a third constituent corresponding to a rare earth RE RE designating a rare earth comprising yttrium (Y), scandium (Se) and lanthanides, or a non-oxide compound of the rare earth RE, namely a carbide, a boride or a rare earth nitride, or corresponding to a mixture of the rare earth RE and a non-oxide compound of the rare earth RE,
• such a material constitutes a non-oxide system in which the silicon has been advantageously replaced by a third component not undergoing active oxidation while maintaining a self-healing liquid phase thanks to the presence of B2O3 and / or the possible formation of a liquid oxide of the third component.
• the material of the invention has a very good refractoriness because the oxide of the third constituent forms, in the complex protective oxide layer containing a hafnium oxide, an oxide, a defined (or intermediate) compound , a solid solution or an over-structure which makes it possible to increase the thermochemical stability of the protective oxide layer.
• the material contains a boride of the third component and Phafnium in metallic form, or in the form of carbide, boride or nitride, or a mixture of several of these elementary bodies and / or these compounds.
• the material contains a nitride of said rare earth RE, said material also containing a hafnium boride and a non-oxide compound of the hafrtium, or a mixture of several of these compounds.
• the boron is not provided independently, it is nevertheless possible to adjust the amount of boron and hafnium. Indeed, by providing hafnium in the form of two compounds, one of which is a boride, it is possible to adjust, on the one hand, the amount of boron with the boride hafnium, and secondly, the amount of hafnium with the second compound which can be in particular a nitride or a carbide.
• the material contains hafnium and a RE rare earth boride or a hafnium carbide and a RE rare earth boride.
• the material may especially contain hafnium and a rare earth boride DyB 4 where Dy corresponds to dysprosium which is a rare earth of the family of lanthanides, or of hafnium carbide and a rare earth boride DyB 4 where Dy corresponds to dysprosium which is a rare earth of the lanthanide family.
• tantalum or a non-oxide compound of tantalum, or niobium or a non-oxide compound of niobium, or zirconium or a non-oxide compound of zirconium, or a mixture of several of these metals and / or compounds may be further added to the three constituents defined above in order to provide a stable additional liquid phase.
• the invention also relates to a refractory part resistant to high temperature in oxidizing medium characterized in that it is made of a refractory material according to the invention.
• the invention also relates to a piece of thermostructural composite material comprising at least in part carbon provided with a high temperature protective coating in an oxidizing medium characterized in that said protective coating consists of a refractory material according to the invention.
• This part may constitute in particular a rocket motor component of composite material C / C whose at least the inner surface is provided with said protective coating.
• the invention also proposes a method for producing a refractory material part resistant to high temperature in an oxidizing medium, characterized in that it comprises producing a composition containing at least:
• a third constituent corresponding to a rare earth RE or a non-oxide compound of the rare earth RE, or corresponding to a mixture of rare earth RE and a non-oxide compound of the rare earth RE, the said composition being devoid of silicon and of silicon compound,
• the invention also relates to a method for producing a high temperature resistant protective layer in an oxidizing medium on a composite material part comprising at least part of carbon, the method comprising the application to the part of a composition containing at least:
• a second component corresponding to boron or a non-boron oxide compound, or corresponding to a mixture of boron and a non-boron oxide compound
• a third constituent corresponding to a rare earth RE or a non-oxide compound of the rare earth RE, or corresponding to a mixture of rare earth RE and a non-oxide compound of the rare earth RE, the said composition being devoid of silicon and of silicon compound, and the densification of said composition
• the composition contains a boride of the third constituent as well as phafnium in metallic form, or in the form of carbide, boride or nitride, or a mixture of several of these metals and / or these compounds. .
• the composition contains a nitride of said rare earth RE, said material also containing a hafnium boride and a non-hafnium oxide compound, or a mixture of several of these compounds.
• the composition contains hafnium and a RE rare earth boride or a hafnium carbide and a RE rare earth boride.
• the composition may especially contain hafnium and a rare earth boride DyB. ; where Dy corresponds to dysprosium which is a rare earth or hafnium carbide and a rare earth boride DyB 4 where Dy corresponds to dysprosium which is a rare earth.
• the composition may contain, in addition to the three components described above, tantalum, or a non-oxide compound of tantalum, or niobium, or a non-oxide compound of niobium, or zirconium or a non-oxide compound of zirconium, or still a mixture of several of these metals and / or compounds.
• the densification of the composition is carried out by flash sintering or spark plasma sintering (SPS).
• FIGS. 1A and 1B are photographs respectively showing a view from above and in partial section of a C / C composite pellet coated with a protective material according to the invention after exposure of the pellet to a high temperature thermal flux in an oxidizing medium,
• FIGS. 2A and 2B are photographs respectively showing a view from above and in partial section of a C / C composite pad covered with a protective material according to the invention; after exposure of the pellet to a heat flux at high temperature in an oxidizing medium,
• FIG. 3 is a photograph showing a top view of a pellet made with a material according to the invention after exposure of the pellet to a high temperature thermal flux in an oxidizing medium
• FIG. 4 is a photograph showing a top view of a pellet made with a material according to the invention after exposure of the pellet to a high temperature thermal flux in an oxidizing medium
• FIG. 5 is a photograph showing a top view of a pellet made with a material according to the invention after exposure of the pellet to a high temperature heat flow in an oxidizing medium.
• the invention proposes a new refractory material capable of withstanding temperatures above 2000 ° C in an oxidizing medium as defined above by forming a structural system generating a protective oxide layer during its use.
• the material of the invention can be used to form refractories intended for use in such conditions as for example heat shields of re-entry vehicles.
• the material of the invention can also be used as a protective coating for parts of thermostructural composite materials containing at least partly carbon, such as C / C composites, intended to be exposed to high temperatures (> 2000 ° C). C) in an oxidizing medium such as in particular the necks of jet engine nozzles or parts of aircraft engines including turbojet engines.
• the refractory material according to the invention contains at least three constituents.
• the first component is hafnium or zirconium, or a non-oxide compound of one of them, or a mixture of two or more of these metals and / or compounds.
• zirconium it is preferably used in a form other than metal because zirconium in metallic form has a low thermal stability.
• the second component is boron or a non-boron oxide compound, or a mixture of them.
• the third constituent corresponds to a rare earth RE, RE designating a rare earth comprising yttrium (Y), scandium (Se) and lanthanides, or to a non-oxide compound of the rare earth RE, namely a carbide, a boride or a rare earth nitride, or a mixture of rare earth RE and a non-oxide RE rare earth compound.
• the rare earth is here preferably used in a form other than metal because, in metallic form, the rare earth has a low thermal stability.
• the atomic ratio between the first component and the third component is strictly greater than 0 and less than or equal to 25 (1st component / 3rd component> 0 and ⁇ 25) while the atomic ratio between the second component and the third component is strictly greater than 0 and less than or equal to 60 (2 nd constituent / 3 rd constituent> 0 and ⁇ 60).
• the material of the invention does not contain silicon or a compound thereof, for example SiC, in order to avoid active oxidation of the material.
• the three constituents indicated above are in a non-oxide form so that the refractory protective material according to the invention forms an initial non-oxide system.
• the material of the invention does not contain oxides already formed, these being generated only during use.
• the oxides initially formed that is to say the oxides already present in the material during its preparation, generally have a high coefficient of expansion and low thermal conductivity and are, therefore, sensitive to thermal shocks.
• the temperature rise of the material will create thermal shocks at these oxides which may cause cracks and / or flaking in the material.
• the Oxides are formed only during temperature rises in use in an oxidizing medium.
• the constituents of the material system will form alone or between they protective oxides allowing the piece or protective coating constituted by the material of the invention to maintain mechanical integrity and refractoriness.
• Hafnium or zirconium are chosen because, as indicated above, they correspond to very good basic constituents for the system formed by the material of the invention in particular because of the high melting temperature of their oxides (from the order of 3000 ° C) and their high resistance to thermal shocks.
• boron oxide B2O3 in liquid form capable of sealing the porosities and cracks that may occur in the protective oxides of hafnium (HfO; ) or zirconium (ZrC).
• the silicon or one of its compounds are absent and advantageously replaced in the protective material of the invention by the third component.
• This third constituent makes it possible to confer and ensure the material a very good refractory nature because the oxide of this third constituent forms, in the protective oxide layer containing a hafnium or zirconium oxide, an oxide, a compound defined (or intermediate), a solid solution or on ⁇ structure that increase the thermochemical stability of the protective oxide layer.
• rare earths capable of forming a non-oxide system with zirconium mention may in particular be made of: lanthanum (La), neodymium (Nd), bromine (Sm), europium (Eu), gadolinium ( Gd), erbium (Er), dysprosium (Dy), lutetium (Lu), ytterbium (Yb), yttrium (Y) and holmium (Ho), and scandium (Se).
• the oxides of these constituents have a melting point above 2000 ° C. They can form compounds defined with B 2 0 3 at a temperature below 2000 ° C. Moreover, at temperatures above 2000 ° C., the oxides of the constituents La, Nd, Sm, Eu, Er, Y have intermediate compounds with Zr0 2 .
• rare earths capable of forming a non-oxide system with hafnium will be mentioned in particular; lanthanum (La), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), erbium (Er), dysprosium (Dy), lutetium (Lu), ytterbium (Yb), yttrium (Y), holmium (Ho) and thulium (Tm).
• the oxides of these constituents have a melting temperature greater than 2000 ° C. They can form compounds defined with B2O3 at a temperature below 2000 ° C. Moreover, at temperatures above 2000 ° C., the oxides of the constituents La, Nd, Sm, Eu, Gd exhibit intermediate compounds with HfO 2.
• the oxide of the third component may be in solid or liquid form and may or may not have low temperature defined compounds with B2O3. Indeed, the existence of compounds defined between the oxide of the added component and the boron oxide at low temperature, may be at the origin of a strong chemical affinity preservation at higher temperature between these two compounds. the liquid state and limit the volatilization of the phase B 2 0 3 .
• tantalum or a non-tantalum oxide compound such as for example TaC, or else niobium or a non-oxide compound of niobium, such as for example NbC, or zirconium or a zirconium compound when it is not not already present in the first component, or a mixture of these metals and / or compounds may be further added to the three components mentioned above to provide an additional stable liquid phase in the system.
• niobium or a non-oxide compound of niobium such as for example NbC
• zirconium or a zirconium compound when it is not not already present in the first component, or a mixture of these metals and / or compounds
• the material according to the invention may in particular be made from a composition comprising a mixture of powders of at least three components described above.
• a composition comprising a mixture of powders of at least three components described above.
• Flash sintering or "SPS"
• SPS Spark Plasma Sintering
• Flash sintering or SPS is a process similar to conventional hot pressing which can also be used to densify the shaped composition.
• Flash sintering consists of a heat treatment under pressure with passage of an electric current which consolidates the part by formation of connection between grains without total melting thereof. This weld made by diffusion of material, is accompanied by a densification, that is to say a decrease in the porosity rate, a hardening and gives cohesion to the shaped object.
• the composition shaped according to that of the part to be produced is introduced into an enclosure for applying a uniaxial pressure during sintering.
• a device for implementing this flash sintering is notably marketed by Sumitomo Electric Industries and makes it possible to subject the sample to pulses (3.3 ms) of continuous electric current (typically 0-10 V, 1-5 kA ) while applying a pressure of several tens of MPa (up to 150 MPa) and this in a range of temperatures varying from the temperature ambient temperature up to 2000 ° C. Flash sintering is usually done under vacuum but it is possible to work under an inert atmosphere (nitrogen, argon).
• the same sintering cycle can be used as a reference for the flash sintering densification of the various compositions of the refractory material according to the invention, only the final sintering temperature is modified as a function of the refraction of the components to be sintered.
• the temperature parameters chosen for the sintering cycle are, for example; a rise to 600 ° C in 3 minutes, followed by a rise to the sintering temperature with a speed of 100 ° C / min, then a plateau at this temperature for 5 minutes and finally a descent to 600 ° C in 30 minutes then the heating stop.
• a pressure of 100 MPa is applied progressively from the beginning of the temperature rise to 600 ° C to close the majority of the remaining pores and avoid densification heterogeneity in the material after sintering.
• a generally dense material can be obtained, for which the contact between the grains is optimal.
• the controlled cooling allows a relaxation of residual stresses of thermal origin and change of structure of the present phases and also to avoid the presence of cracks and microcracks in the material.
• Examples of sintering atmosphere, melting temperature values and sintering temperature for some of the constituents of the composition of materials according to the invention are shown in the table below.
• the molds and pistons used are graphite and are separated from the composition in powder form compacted by a graphite sheet to prevent sticking.
• thermostructural composite material for example C / C
• the C / C composite part is placed in the sintering mold on a bed of powder (corresponding to the mixture of powders constitutive constituents of the material of the invention), then is covered with the same powder to be completely in the center of the piece formed by flash sintering.
• a bed of powder corresponding to the mixture of powders constitutive constituents of the material of the invention
• the monolithic parts and protective coatings of refractory material resistant to high temperature in an oxidizing medium according to the invention can also be produced by standard sintering or by plasma spraying or by vapor deposition (PVD).
• the following two tables show examples of compactness and phases identified by X-ray diffraction in materials obtained from different powder compositions densified by flash sintering under the operating conditions described above and with the indicated sintering temperature. in the tables.
• the samples thus produced are then tested for oxidation in ambient air in a solar oven where they are subjected to a solar flux of 15.5 MW.m 2 for a duration of plateau at maximum temperature of 3 minutes.
• Tcn, m, Ec and Eo respectively correspond to the value of the exposure black body temperature, to the indication of the mass variation, to the value of the thickness of material consumed and to the value of the thickness of the oxidized layer of the material Hf + DyB 4 on composite C / C.
• Tcn, ⁇ , Ec and Eo respectively correspond to the value of the exposure black body temperature, to the indication of the mass variation, to the value of the material thickness consumed and to the value of the thickness of the oxidized layer of the material HfC + DyB 4 on composite C / C.
• Tcn, ⁇ , Ec and Eo respectively correspond to the value of the exposure black body temperature, to the indication of the mass variation, to the value of the material thickness consumed and to the value of the thickness of the oxidized layer of the material Hf + GdB,;
• Tcn, ⁇ , Ec and Eo respectively correspond to the value of the exposure black body temperature, to the indication of the mass variation, to the value of the thickness of material consumed and the value of the thickness of the oxidized layer of the material HfC + GdB 6 .
• FIG. 5 show the results obtained for a sample comprising a monolithic pellet made of ZrC + GdB 6 material (2.7), the sample having been formed and tested under the conditions described above.
• Tcn, ⁇ , Ec and Eo respectively correspond to the value of the exposure black body temperature, to the indication of the mass variation, to the value of the material thickness consumed and to the value of the thickness of the oxidized layer of ZrC + GdB 6 material .
• This liquid phase can fill the porosities at the extreme surface of the porous refractory skeleton of HfCb at a black body temperature of at least 2150 ° C. or a real temperature greater than 2300 ° C.
• the diffusion of oxygen through the oxide layer can be limited.

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