WO2019123223A1 - Procédé de fabrication d'une préforme poreuse en carbure de silicium ayant une porosité contrôlée et préforme poreuse en carbure de silicium - Google Patents

Procédé de fabrication d'une préforme poreuse en carbure de silicium ayant une porosité contrôlée et préforme poreuse en carbure de silicium Download PDF

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WO2019123223A1
WO2019123223A1 PCT/IB2018/060216 IB2018060216W WO2019123223A1 WO 2019123223 A1 WO2019123223 A1 WO 2019123223A1 IB 2018060216 W IB2018060216 W IB 2018060216W WO 2019123223 A1 WO2019123223 A1 WO 2019123223A1
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preform
silicon carbide
porosity
aluminium
heat treatment
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PCT/IB2018/060216
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English (en)
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Mattia ALEMANI
Mario Tironi
Giuseppe MAGNANI
Federica BURGIO
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Freni Brembo S.P.A.
ENEA - Agenzia nazionale per le nuove tecnologie, l'energia e lo sviluppo economico sostenibile
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Priority to CN201880086610.4A priority Critical patent/CN111868008B/zh
Publication of WO2019123223A1 publication Critical patent/WO2019123223A1/fr

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    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D65/00—Parts or details
    • F16D65/02—Braking members; Mounting thereof
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
    • C04B2235/6585—Oxygen containing atmosphere, e.g. with changing oxygen pressures at an oxygen percentage above that of air
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D2200/00—Materials; Production methods therefor
    • F16D2200/0082—Production methods therefor

Definitions

  • the present invention relates to a method of making a porous preform in silicon carbide with controlled porosity and a silicon carbide porous preform, in particular obtained with such method.
  • the porous preform of silicon carbide according to the invention is capable of being infiltrated with aluminium or alloys thereof for the manufacture of components of braking systems, in particular disc brake bands, made of MMC (Metal Matrix Composite) .
  • MMC Metal Matrix Composite
  • silicon carbide is among the most promising ceramic materials for applications both at ambient temperature and at high temperature (up to approximately 1500°C) .
  • silicon carbide has low specific weight, high hardness, high elastic modulus, low tenacity and high resistance to oxidation and corrosion. Due to these characteristics, silicon carbide is used even for structural components operating in extreme conditions or for manufacturing porous components such as filters and membranes.
  • the known process consists of thermally treating silicon carbide powder at a lower temperature than the traditional sintering temperature, 2100-2200°C. Treating in a vacuum at 1700- 2000°C the SiC powder without additives, Jang et al . were able to obtain porous specimens with maximum porosity of 40% (J. Alloys Compd., 463, 493-497 (2008)).
  • the partial sintering method is the simplest and most economical one for obtaining porous specimens with maximum porosity of approximately 65% as stressed by Eom et al . in Journal of Asian Ceramic Societies, 1, 220-242 (2013) .
  • the main limit of this method is that to obtain specimens with high porosity (>40%) it is necessary to use secondary phases that must be added to the commercial SiC powders with consequent additional process costs, reproducibility problems and possible compromising of the properties of the final component because of the presence of these secondary phases .
  • the methods based on the use of sacrificial templates, of replications and of foaming agents are particularly suited for obtaining high porosity components, even up to 95%, but they also require mixing SiC powders with specific substances that allow reaching these levels of porosity.
  • the main limit of these methods is the difficulty of assuring high reproducibility, especially in the case of production of large series of large-sized components. It also has a higher cost because of the complexity of the process.
  • the silicon carbide powder is mixed with graphite or with graphite/alumina and is then sintered in air at a maximum temperature of 1500°C to promote the formation of silicon (in the presence of graphite) or mullite (in the presence of graphite/alumina) .
  • This methodology was proposed by She et al . in "Oxidation bonding of porous silicon carbide ceramics"- J. Mater. Sci., 37, 3615-3622 (2002) and is based on the formation of a glassy phase among the particles of SiC.
  • a porous component having maximum porosity of approximately 45% vol. is obtained.
  • the final component will consist of a mixture of silicon carbide and bonding agent in the form of glassy phase that compromises the properties of the material.
  • a process for fabricating MMC starting from a porous preform of silicon carbide is disclosed in the patent US 6,186,768 B1 of 2001.
  • the porous preform is made of recrystallized SiC (max porosity 40% vol), obtained at a temperature above 2200°C, using a mixture of SiC powders at different granulometry.
  • the fine powder sublimating allows to obtain the bonds between the largest powder particles creating an open porosity network .
  • the MMC composite is obtained starting from a preform of recrystallized SiC obtained mixing powders at different granulometry and treating the mixture in the temperature range of 1900- 2400°C.
  • the preform has a max porosity of 30%.
  • porous preforms made of ceramic material with porosities above 70% are to be obtained, it is necessary to use appropriate porosity- inducing additives to be added to the powder of the ceramic material.
  • porous preforms made of ceramic material having the possibility of controlling the final porosity of the preform and of obtaining porosities above 60% without using porosity-inducing additives.
  • said method comprising the following operating steps:
  • Each heat treatment cycle comprises in sequence:
  • a porous preform in at least partly sintered silicon carbide is obtained with a final porosity f3 higher than the intermediate porosity f2 of said sintered preform.
  • Each heat treatment cycle causes a progressive increase of the porosity of said preform.
  • the number of heat treatment cycles to be performed on said pre sintered preform is defined as a function of the value of final porosity f3 to be obtained in the porous preform of at least partially sintered silicon carbide so as to control the final porosity value f3 of the porous preform.
  • the final porosity f3 to be obtained of the porous preform in at least partly sintered silicon carbide increases substantially linearly as the number of said heat treatment cycles increases, starting from the initial porosity value f ⁇ of the semi-finished preform.
  • the number of heat treatment cycles to be carried out on said pre-sintered preform is predefined as a function of the final porosity value f3 to be obtained in the porous preform of at least partly sintered silicon carbide on the basis of experimental curves that relate the final porosity f3 of the porous preform in at least partly sintered silicon carbide with the number of said heat treatment cycles, once the initial porosity value f ⁇ of the semi-finished preform is established .
  • the aforesaid forming step a) is conducted by means of uniaxial pressing or by cold isostatic pressing of the mass of silicon carbide powders.
  • the initial porosity value f ⁇ of the semi finished preform decreasing as the pressure at which the forming is conducted increases.
  • the aforesaid forming step a) is conducted by moulding said mass of silicon carbide powders in aqueous suspension, preferably by means of the slip casting technique.
  • the initial porosity value f ⁇ of the semi-finished preform decreasing as the content by volume of said powders in the aqueous suspension increases .
  • the aforesaid silicon carbide powders are made from silicon carbide granules coated on the surface with a polymeric binder composition.
  • the polymeric binder composition is selected from the group consisting of phenolic resins, PEG and PVA.
  • the aforesaid silicon carbide powders made from silicon carbide granules coated on the surface with a polymeric binder composition comprise sintering additives, preferably carbon and boron carbide.
  • the method comprises a step d) of thermally eliminating from said semi-finished preform the organic components of the polymeric binder composition coating the granules of silicon carbide powder.
  • Said elimination step d) is conducted after said forming step a) and before said pre sintering step b) , in an inert atmosphere or in air at a temperature between 250°C and 900°C, preferably between 300°C and 800°C and even more preferably between 350°C and 700 ° C .
  • the method comprises a final sintering step e) , conducted in an inert atmosphere after said one or more heat treatment cycles c) at a temperature above 2,000°C, preferably at a temperature which can reach the sublimation temperature of silicon carbide, even more preferably up to a temperature of about 2,200°C.
  • Said sintering step e) leaves unchanged the final porosity f3 of the preform.
  • the aforesaid step b) of pre-sintering said semi-finished preform is conducted for a time period of at least a few seconds up to a maximum of 60 minutes.
  • step b) of pre sintering said semi-finished preform is conducted at a temperature in the range of 1,700°C to 1,900°C, and preferably in the range of 1,750°C to 1,850°C.
  • the oxidation sub-step cl) of each heat treatment cycle c) is conducted for a period of time between 30 and 120 minutes.
  • the oxidation sub-step cl) of each heat treatment cycle c) is conducted at a temperature in the range of 800°C to 1,200°C, and preferably in the range of 1, 000°C to 1, 150 °C .
  • the partial sintering sub-step c2) of each heat treatment cycle c) is conducted for a period of at least a few seconds, up to a maximum of 60 minutes.
  • the partial sintering sub-step c2) of each heat treatment cycle c) is conducted at a temperature in the range of 1,700°C to 1,900°C, and preferably in the range of 1,750°C to 1,850°C.
  • each partial sintering sub-step c2) of each heat treatment cycle c) is conducted in an oven in a carbonaceous atmosphere.
  • An object of the present invention is a silicon carbide porous preform obtained with the method according to the invention.
  • An object of the present invention is a silicon carbide porous preform constituted of at least 99% by weight of silicon carbide, which can have a content of metal impurities not exceeding 1% by weight, and having a porosity above 60% by volume.
  • An object of the present invention is also a method of making a component constituted at least in part of an aluminium-based metal matrix composite reinforced by a porous preform of at least partly sintered silicon carbide .
  • Said method comprises the following operating steps:
  • said silicon carbide porous preform has a porosity of not lower than 60% in volume, and preferably between 60% and 65% in volume.
  • the step d) of infiltrating aluminium or an aluminium alloy is conducted using the technique of infiltration in the semi-solid state.
  • the aforesaid preform occupies only a part of said mould.
  • the part of said mould not occupied by the preform is filled with aluminium or aluminium alloy.
  • the component is thus constituted of a first part in aluminium-based metal matrix composite reinforced by said preform and of a second part in cast aluminium or aluminium alloy. Said two parts form a co cast one piece.
  • the aforesaid component is a brake disc.
  • the first part defines at least partially the braking band of the brake disc and the second part defines at least the bell of the brake disc.
  • An object of the present invention is an aluminium- based metal matrix composite reinforced with a sintered silicon carbide porous preform, obtained with the method according to the invention.
  • An object of the present invention is a component made at least in part of an aluminium-based metal matrix composite reinforced with a sintered silicon carbide porous preform.
  • agglomerates of granules of silicon carbide (SiC) having a uniform average size, preferably not higher than 100 pm, are evenly distributed.
  • the aforesaid metal matrix composite consists of 39% to 44% by weight of silicon carbide (SiC) and of 56% to 61% by weight of aluminium or aluminium alloy metal matrix.
  • the aforesaid component is a component of a braking system, in particular of a disc braking system.
  • said component is a braking band of a brake disc, a brake disc calliper or a portion of a brake disc.
  • FIG. 1 shows the pattern of the density of porous preforms made of SiC according to a preferred embodiment of the invention, with respect to the values of the pressure exerted in a forming step; the density is expressed as % of the theoretical density of the SiC; the Figure shows different patterns parameterized on the number of cycles of oxidation / partial sintering, to which the preforms were subjected;
  • FIG. 2 shows the pattern of the density of porous preforms made of SiC according to a preferred embodiment of the invention, with respect to the values of the pressure exerted in a forming step; the density is expressed as % of the theoretical density of the SiC; the Figure shows different patterns parameterized on the values of the pressure exerted in a forming step of the individual preform;
  • the method according to the invention for making a porous preform in silicon carbide with controlled porosity comprises the following steps:
  • a porous preform in at least partly sintered silicon carbide is obtained with a final porosity f3 higher than the intermediate porosity f2 of the aforesaid sintered preform.
  • Each heat treatment cycle causes a progressive increase of the porosity of the aforesaid preform, as will be clarified in the description .
  • the number of heat treatment cycles to be performed on the aforesaid pre-sintered preform is defined as a function of the value of final porosity f3 to be obtained in the porous preform of at least partially sintered silicon carbide so as to control the final porosity value f3 of the porous preform.
  • the term "porosity" f means the portion of volume of the preform available to be filled by the liquid metal.
  • the porosity f of the porous preform is expressed as % value of the volume of the preform. Said value of porosity f is calculated indirectly from the geometric density of the preform, expressed as % of the theoretical density of silicon carbide (equal to 3.2 g/cm3) . It is possible to take as a reference the theoretical density of silicon carbide since the preforms obtained with the method according to the invention are substantially constituted only by silicon carbide.
  • Porosity f expressed as % over the theoretical density of silicon carbide, is calculated as the difference between the theoretical density expressed as a % value (100%) and the geometric density of the preform expressed as %. For example, a preform having a geometric density of 40% of theoretical density has a porosity of 60%.
  • the method according to the invention allows to make porous preforms of silicon carbide, obtaining final porosities f3 even higher than 60% (density ⁇ 40%) without the use of porosity-inducing additives.
  • the porous preforms obtained according to the invention are constituted substantially only by silicon carbide, lacking secondary phases, to the advantage of the homogeneity of the material.
  • the method according to the invention allows to obtain preforms with porosity values above 60%, lacking secondary phases, using common ovens operating in controlled atmosphere and not necessarily ovens operating in a vacuum. This constitutes a significant advantage in terms of reduction of plant and process costs.
  • the method according to the invention also allows to adjust the value f3 of the final porosity of the preform, acting on the initial value f ⁇ of the semi-finished preform and on the number of heat treatment c) cycles carried out.
  • the method thus allows to increase the porosity of silicon carbide preforms in a progressive and controlled manner. This constitutes a significant advantage in terms of controllability and reproducibility of the productive process.
  • the method according to the invention can also be used to produce porous preforms with low porosity, and not only with high porosity. Concerning the definition of the final porosity of the preforms, the method according to the invention is very flexible because it allows to obtain porous preforms of silicon carbide having final porosity values that can be selected in a very broad range of values. In particular, this interval of choice of porosity can extend from 5% to 75%.
  • the number of heat treatment cycles to be carried out on the aforesaid pre-sintered preform can be predefined as a function of the final porosity value f3 to be obtained in the porous preform of at least partly sintered silicon carbide, once the initial value of porosity f ⁇ of the semi-finished preform is set, on the basis of predefined experimental curves that relate the final porosity f3 of the porous preform with the number of the heat treatment cycles.
  • the aforesaid experimental curves, parameterized on the initial value of porosity f ⁇ of the semi-finished preform, have a substantially linear pattern. It has been possible to verify experimentally that the final porosity f3 to be obtained of the porous preform in silicon carbide increases substantially linearly as the number of said heat treatment cycles increases, starting from the initial porosity value f ⁇ of the semi-finished preform.
  • the average slope of the curve with linear pattern depends on the temperatures and on the execution times of the two sub-phases cl) and c2) .
  • porous preforms of silicon carbide can thus be obtained, assuring the possibility of controlling and predicting the final porosity of the preform.
  • the method according to the invention thus allows to implement a productive process that is simple and economical to carry out.
  • the forming step a) can be conducted with any technique .
  • the forming step a) is conducted by means of uniaxial pressing or by cold isostatic pressing of the mass of silicon carbide powders.
  • the initial porosity value f ⁇ of the semi-finished preform decreasing as the pressure at which the forming is conducted increases.
  • the parameter for adjusting the initial porosity f ⁇ of the semi-finished preform thus consists of the forming pressure.
  • the forming step a) can be conducted by moulding the aforesaid mass of silicon carbide powders in aqueous suspension, preferably by means of the slip casting technique .
  • the initial porosity value f ⁇ of the semi-finished preform decreasing as the content by volume of the powders in the aqueous suspension increases.
  • the parameter for adjusting the initial porosity f ⁇ of the semi-finished preform thus consists of the volume content of the powders in the aqueous suspension.
  • the powder of silicon carbide is dispersed in a liquid (water or organic solvent) with the aid of a dispersant and cast inside a chalk mould.
  • the forming technique is selected according to the type of preform to be obtained.
  • Uniaxial pressing is the most economical technique and it is suitable to obtain preforms with simple shape and for industrial series productions. If it is necessary to form complex preforms, other forming techniques can alternatively be used, and in particular isostatic pressing, slip casting, injection moulding. Ready-to- press powders are specific for uniaxial and isostatic pressing
  • the method according to the invention is applicable to silicon powders that are highly different from each other in terms of granulometry .
  • the aforesaid silicon carbide powders used in the forming step a) are made from silicon carbide granules coated on the surface with a polymeric binder composition.
  • coated powder hereinafter, reference will generally be made to "coated powder" .
  • the presence of the polymeric binder composition is functional to give cohesion to the mass of powders after the forming step a) and before the pre sintering step b) , so as to make the semi-finished preform manipulable.
  • the polymeric binder composition that superficially coats the granules of silicon carbide powders is selected from the group consisting of phenolic resins, polyethylene glycol (PEG) and polyvinyl alcohol (PVA) .
  • PEG polyethylene glycol
  • PVA polyvinyl alcohol
  • the choice of a specific binding polymeric composition is not essential.
  • the method according to the invention is applicable to powders coated with any type of polymeric composition.
  • the forming step a) is conducted by means of uniaxial pressing or by cold isostatic pressing of the mass of silicon carbide powders.
  • the forming step a) is conducted at a moulding pressure in the range of 0.1 - 1 t/cm2, preferably in the range of 0.2-0.6 t/cm2, and even more preferably in the range of 0.3-0.5 t/cm2.
  • the value of the forming pressure is selected as a function of the initial porosity value f ⁇ to be obtained in the semi-finished preform and of the powder used.
  • "ready-to-press" powders containing carbon and boron carbide are used as sintering additives.
  • Boron can be used instead of boron carbide.
  • Aluminium and aluminium carbide can also be used.
  • an aggregate is obtained of the aforesaid silicon carbide granules mutually connected by connecting ceramic microstructures generated by the respective coatings of binding polymeric composition.
  • This aggregate contains organic residues deriving from the coatings of the granules.
  • the method also comprises a step d) of thermally eliminating from said semi-finished preform obtained at the end of the step a) of forming the organic components of the binding polymeric composition that coats the granules of the silicon carbide powders.
  • Said step d) of eliminating the organic residues (hereafter also called dewaxing step) is carried out in inert atmosphere or in air, after the aforesaid forming step a) and before the pre-sintering step b) .
  • the temperature at which the dewaxing step d) is carried out depends on the type of organic residues to be eliminated.
  • the step d) of eliminating the organic residues (dewaxing) is conducted at a temperature between 250°C and 900°C, preferably between 300°C and 800°C, and still more preferably between 350°C and 700°C.
  • the step d) of eliminating the organic residues (dewaxing) is protracted until the complete elimination of the organic phase present in the mass of silicon carbide granules after forming.
  • the step d) of eliminating the organic residues (dewaxing) is preferably carried out under an air flow.
  • the step d) of eliminating organic residues (dewaxing) allows not only to eliminate the bonding agents, but also to oxidise the silicon carbide powders thus blocking the sintering of the preform that would be facilitated by the presence of the sintering additives.
  • the step d) of eliminating the organic residues (dewaxing) is preferably carried out in an inert atmosphere. In this case, there is no tendency to sintering and oxidation of the powders is not necessary. In this case, the step d) of eliminating organic residues (dewaxing) is thus functional only to eliminate the bonding agents.
  • the method according to the invention is also applicable to coated silicon carbide (i.e. not superficially coated by a binding polymeric composition) , although this can lead to greater difficulties in the step a) of forming the powders.
  • the semi-finished preform is subjected to the pre-sintering step b) .
  • the purpose of the pre-sintering step b) is to consolidate the semi-finished preform, transforming it in a continuous structure with homogeneous mechanical characteristics .
  • the pre-sintering step b) is conducted assuring a minimum and homogenous contraction of the semi-finished preform in order to maintain the dimensional characteristics of the preform.
  • the pre-sintering step b) nevertheless causes a contraction of the semi-finished preform and a correlated increase in porosity (i.e. a decrease in density, calculated as % of the theoretical density of silicon carbide) .
  • the (pre-sintered) preform has an intermediate porosity f2, lower than the initial porosity f ⁇ .
  • the aforesaid pre-sintering step b) is conducted at a temperature in the range of 1,700°C to 1,900°C, and preferably in the range of 1,750°C to
  • the preform has insufficient mechanical characteristics. At lower temperatures, the preform is progressively less oxidizable .
  • the aforesaid pre-sintering step b) is conducted for a time period of at least a few seconds (preferably at least 2 seconds of permanence at the selected pre-sintering temperature) , up to a maximum of 60 minutes.
  • the time duration is correlated to the temperature at which the process is carried out, with a view to cost containment.
  • the method according to the invention envisages that the pre-sintered preform is subjected to one or more heat treatment cycles c) , where each heat treatment cycle comprises in sequence:
  • a porous preform in at least partly sintered silicon carbide is obtained with a final porosity f3 higher than the intermediate porosity f2 of the aforesaid sintered preform.
  • Each heat treatment cycle causes a progressive increase of the porosity of the aforesaid preform, but without causing dimensional changes of the preform.
  • each oxidation sub phase cl is to progressively consume the silicon carbide, creating an ever greater porosity.
  • the chemical phenomenon that occurs can be schematically represented as follows:
  • the subsequent partial sintering sub-phase c2) which is preferably conducted in the presence of free carbon inside the oven where it is conducted (carbonaceous atmosphere) allows the transformation of the silica (Si02) into silicon carbide (SiC) .
  • each sintering sub-phase (c2) is carried out inserting carbon elements inside the oven, in particular graphite crucibles, preferably coated with graphite sheets.
  • SiC is formed on the graphite elements present in the oven, and hence externally to the preform. Thus, all this occurs without dimensional changes of the preform. Density drops because the weight decreases. Operatively, since the preform is porous, it oxidises homogeneously. Consequently, the preform is "consumed" homogeneously involving the whole volume and not preferentially from the exterior towards the interior.
  • the oxidation sub-step cl) of each heat treatment cycle c) is conducted at a temperature in the range of 800°C to 1,200°C, and preferably in the range of 1, 000°C to 1,150°C. It has been observed experimentally that for temperatures below 800°C the oxidation is minimal. For temperatures above 1200°C, oxidation could be excessive, causing the rupture of the preform in the subsequent partial sintering sub phase c2 ) .
  • the oxidation sub-step cl) of each heat treatment cycle c) is conducted for a period of time between 30 and 120 minutes.
  • the partial sintering sub-step c2) of each heat treatment cycle c) is conducted at a temperature in the range of 1,700°C to 1,900°C, and preferably in the range of 1,750°C to 1,850°C.
  • the preform has insufficient mechanical characteristics.
  • the preform is progressively less oxidizable.
  • the partial sintering sub-step c2) of each heat treatment cycle c) is conducted for a period of at least a few seconds, up to a maximum of 60 minutes.
  • the time duration is relevant from the viewpoint of costs, in that containing times is advantageous especially at these temperature levels.
  • the selection of the duration of the sub-phases Cl) and c2) depends on temperature. The higher the temperature, the less time is necessary for oxidation and partial sintering.
  • the time duration parameter is relevant, together with temperature, because depending on the mix of these two parameters a straight line is substantially obtained with different slope in the number of cycles/density chart.
  • the porous preform of silicon carbide obtained at the end of the aforesaid one or more heat treatment cycles c) can be subjected to a final sintering step e) that is conducted in inert atmosphere at a temperature above 2,000°C, and that in particular can reach the sublimation temperature of silicon carbide, preferably at a temperature of approximately 2,200°C.
  • Said final sintering allows to improve the mechanical resistance properties (in particular, flexural strength) and at the same time to increase the oxidation resistance of the porous preform of at least partially sintered silicon carbide.
  • final sintering thus also has the purpose of stabilising the porous preform of at least partially sintered silicon carbide, making it insensitive to any subsequent oxidations that the preform could subsequently undergo.
  • BSSM infiltration comprises a step of pre-heating the porous preform.
  • the method according to the invention - in the preferred case in which a final sintering step is envisaged - then allows to obtain preforms even with very high porosities (very low densities) that can be subjected to temperatures above 2000°C in inert atmosphere without undergoing changes to their internal porous structure.
  • step a) of the method according to the invention Approximately 27 grams of ready-to-press silicon carbide powder STARCERAM RQ produced by H.C. Starck GmbH were placed inside a cylindrical mould with 40 mm diameter and they were pressed at different pressures (step a) of the method according to the invention) : 0.15 t/cm2, 0.2 t/cm2, 0.3 t/cm2 and 0.6 t/cm2. The density of these samples was determined geometrically weighing them with an analytical scale with sensitivity ⁇ 0.0001 g and measuring their height and diameter with a comparator with sensitivity ⁇ 0.01 mm.
  • step e The cylindrical samples obtained at the end of moulding (green samples, green body) were then placed in an oven and heat treated in flowing air at 350°C with stasis at this temperature of 1 h (step e) of eliminating organic residues - dewaxing) . Subsequently, the samples were pre sintered in inert atmosphere (argon) at 1800°C for a time of 2 seconds (pre-sintering step b) of the method) . The densities of the pre-sintered samples were determined geometrically according to the procedure described above. These pre-sintered samples were then subjected to 6 series of cycles of oxidation and partial sintering (step c) of heat treatment of the method) .
  • the oxidation (sub phase cl) was carried out in flowing air at 1100°C with stasis at this temperature of 1 h, while the partial sintering (sub-phase c2) was always carried out at 1800°C in carbonaceous atmosphere.
  • the carbonaceous atmosphere was obtained by placing graphite sheets inside graphite crucibles. Silicon carbide (SiC) is formed on the graphite sheet and on the walls of the crucible .
  • Figure 1 shows the pattern of the density of the porous preforms made of partially sintered SiC, with respect to the values of the pressure exerted in the forming step; the Figure shows different patterns parameterized on the number of cycles of oxidation / partial sintering, to which the preforms were subjected.
  • Figure 2 shows the pattern of the density of the same porous preforms of Figure 1, with respect to the number of cycles of oxidation / partial sintering, to which the preforms were subjected.
  • the Figure shows different patterns parameterized on the values of the pressure exerted in the forming step of the individual preform.
  • the porosity f of the sample (porous preform) is calculated as % value expressed by the difference between theoretical density of silicon carbide (unit reference value, 100%) and % density of the preform.
  • pre sintered samples were then subject to an oxidation and partial sintering cycle (heat treatment step c) .
  • the oxidation was carried out in flowing air at 1100°C with stasis at this temperature of 1 h, while the pre sintering was carried out at 1800°C with a time of permanence at that temperature of 2 seconds.
  • All preforms were then heat treated at 2200°C (step d) of final sintering.
  • the experimental results are shown in Table 3.
  • An object of the present invention is a silicon carbide porous preform obtained with the method according to the invention, and in particular as described above.
  • An object of the present invention is a silicon carbide porous preform constituted of at least 99% by weight of silicon carbide, which can have a content of metal impurities not exceeding 1% by weight, and having a porosity above 60% by volume.
  • the porous preform of silicon carbide has no secondary phases and hence has high composition homogeneity.
  • An object of the present invention is also a method of making a component constituted at least in part of an aluminium-based metal matrix composite reinforced by a porous preform of silicon carbide.
  • said method comprises the following operating steps:
  • the aforesaid silicon carbide porous preform has a porosity of not lower than 60% in volume, preferably between 60% and 65% in volume.
  • the aforesaid porous preform was subjected to a final sintering step d) , envisaged as an optional step in the method for producing porous preforms according to the invention.
  • the porous preform is made capable of withstanding any oxidative phenomena that can be induced by the infiltration process and hence capable of maintaining its morphological characteristics substantially unaltered.
  • the step of infiltrating with aluminium or aluminium alloy of the porous preform can be carried out by different techniques.
  • the infiltration techniques usable in the present invention can be divided in two macro-categories: “liquid infiltration” and “pressure infiltration”. In both cases the alloy used is in the liquid state, but the pressure at which said alloy is injected changes.
  • This first family (“liquid infiltration”) comprises :
  • [00181] - centrifugal casting it is similar to gravity casting, but with the addition of centrifugal forces due to the rotation of the casting system;
  • [00182] - pressureless infiltration it implies long infiltration times in a protected atmosphere (typically nitrogen) at temperatures between 700°C and 800°C. Also the pressureless infiltration techniques needs subsequent plastic deformation operations.
  • squeeze casting is in the second category ("pressure infiltration”) .
  • squeeze casting allows the solidification of liquid aluminium, injected into a mould, under pressure.
  • This technology is described in particular in the patent US20140272451 Al, with particular reference to the manufacture of a brake disc with reinforced braking band.
  • the step of infiltrating with aluminium or an aluminium alloy is conducted using a semi-solid infiltration technique.
  • the semi-solid infiltration technique preferably used in the present invention is described in US 2014/0182806 Al, with particular reference to the steps of preparing the alloy, and of injecting it.
  • This process can be generalised on any product with complex geometry after appropriately setting the fundamental parameters such as solid fraction, injection temperature, injection speed, injection pressure and multiplication pressure.
  • the semi-solid infiltration technique envisages that the porous preform of silicon Carbide is heated to a temperature between 600°C and 900°C, and positioned inside the mould into which the semi-solid aluminium will be injected. This will be carried out shortly before completion of the step of mixing the alloy, so that the temperature of the preform does not decrease significantly. Once the mould is closed, the injection subsequently takes place.
  • a porous preform with high porosity is particularly preferred if a semi-solid infiltration technique is adopted.
  • a high porosity of the preform allows to increase the capacity of infiltration of semi-solid aluminium, exploiting a lower resistance to the semi-solid front.
  • the semi-solid state of the metal also reduces the probability of chemical reactions at the SiC/Al interface.
  • the aforesaid preform occupies only a part of the mould.
  • the part of the mould not occupied by the preform is filled with aluminium or aluminium alloy.
  • the component is thus constituted of a first part in aluminium-based metal matrix composite reinforced by the preform and of a second part in cast aluminium or aluminium alloy. The two parts form a co-cast one piece.
  • the invention allows to overcome the limits of standard aluminium alloys, adding a reinforcement only when necessary to improve the mechanical characteristics of the material.
  • the component is a brake disc
  • the part that needs reinforcement can in particular be the braking band.
  • the aforesaid component is a brake disc, in which the aforesaid first part defines at least partially the braking band of the brake disc and the second part defines at least the bell of the brake disc.
  • An object of the present invention is a component made at least in part of an aluminium-based metal matrix composite reinforced with an at least partially sintered silicon carbide porous preform.
  • agglomerates of granules of silicon carbide (SiC) are evenly distributed and have a uniform average sizes.
  • the agglomerates of granules of silicon carbide have a maximum size no greater than lOOpm.
  • Figure 4 shows a scanning electron microscope (SEM) photograph of an MMC Al/SiC material obtained by infiltration with molten silicon of a porous preform of SiC made according to the present invention. From the photograph it is possible to observe that the macrostructure of the aluminium or aluminium alloy metal matrix has granules of silicon carbide (SiC) , evenly distributed and having uniform average sizes (in the specific case, maximum size no greater than 10 pm) .
  • SiC silicon carbide
  • Figure 3 shows a scanning electron microscope (SEM) photograph of a commercially available MMC Al/SiC material published by Liu et al . «Pressureless infiltration of liquid aluminum alloy into SiC preforms to form near-net-shape SiC/Al composites", Journal of Alloys and Compounds 465 (2008) 239-243.
  • the aforesaid metal matrix composite consists of 39% to 44% by weight of silicon carbide (SiC) and of 56% to 61% by weight of aluminium or aluminium alloy metal matrix.
  • the remaining 40% by volume is constituted by SIC with density 3.2 g/cm3.
  • 60% by volume thus consists of aluminium with density 2.7 g/cm3.
  • the metal matrix composite consists of 44% by weight of SiC and of 56% by weight of A1.
  • the aforesaid component is a component of a braking system, in particular of a disc braking system. More in particular, the aforesaid component is a braking band of a brake disc, a brake disc calliper or a portion of a brake disc.
  • the component can consist of any structural components in general.
  • the component can be a filter for gases and liquids.
  • the method according to the present invention is particularly advantageous in the production of preforms with high porosity if "ready-to-press" SiC powders, i.e. containing sintering additives, are used. In this way it is easier to maintain the forming pressure low (no higher than 1.0 t/cm2) . Maintaining a low forming pressure allows to have a low initial density and hence a high starting porosity.
  • the method according to the invention allows to block the tendency to sinter of ready-to-press powders. Due to the invention it is thus possible to use ready-to-press powders to obtain porous preforms with high reproducibility.
  • the SiC preforms obtained according to the invention have a microstructure that maintain "memory" of the starting agglomerates .
  • the sintering additives present in ready-to- press powders are not present in such quantities as to create secondary phases that can contaminate the preforms of silicon carbide.
  • sintering additives create mainly boron carbide at a maximum quantity of 1% by weight. This value refers to sintered preforms with high density.
  • boron carbide B4C probably oxidises in the various steps and hence, if present, a sharply lower content than the aforesaid nominal value can be hypothesised.

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Abstract

La présente invention concerne un procédé de fabrication d'une préforme poreuse en carbure de silicium ayant une porosité contrôlée. Le procédé comprend les étapes opératoires suivantes : - a) formation d'une masse de poudres de carbure de silicium dans un moule obtenant une préforme semi-finie ayant une porosité initiale ϕ1 - b) préfrittage de ladite préforme semi-finie dans une atmosphère inerte à une température dans la plage de 1 600 °C à 2 000 °C, obtention d'une préforme préfrittée ayant une porosité intermédiaire (ϕ2) supérieure à la porosité initiale (ϕ1) ; - c) soumission de ladite préforme préfrittée à un ou plusieurs cycles de traitement thermique. Chaque cycle de traitement thermique comprend, en séquence : - une sous-phase c1) d'oxydation dans l'air à une température dans la plage de 700 °C à 1 250 °C ; et-une sous-phase c2) de frittage partiel à une température dans la plage de 1 600 °C à 2 000 °C. Après l'étape mentionnée ci-dessus c) une préforme poreuse en carbure de silicium au moins partiellement fritté est obtenue ayant une porosité finale ϕ3 supérieure à la porosité intermédiaire ϕ2 de ladite préforme frittée. Chaque cycle de traitement thermique provoque une augmentation progressive de la porosité de ladite préforme. Le nombre de cycles de traitement thermique à effectuer sur ladite préforme préfrittée est défini en fonction de la valeur de porosité finale ϕ3 à obtenir dans la préforme poreuse de carbure de silicium au moins partiellement fritté de façon à contrôler la valeur de porosité finale ϕ3 de la préforme poreuse.
PCT/IB2018/060216 2017-12-20 2018-12-18 Procédé de fabrication d'une préforme poreuse en carbure de silicium ayant une porosité contrôlée et préforme poreuse en carbure de silicium WO2019123223A1 (fr)

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