EP3687958A1 - Composant céramique - Google Patents

Composant céramique

Info

Publication number
EP3687958A1
EP3687958A1 EP18782380.2A EP18782380A EP3687958A1 EP 3687958 A1 EP3687958 A1 EP 3687958A1 EP 18782380 A EP18782380 A EP 18782380A EP 3687958 A1 EP3687958 A1 EP 3687958A1
Authority
EP
European Patent Office
Prior art keywords
green body
carbon
resin
ceramic component
component according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP18782380.2A
Other languages
German (de)
English (en)
Inventor
Andreas Kienzle
Dominik RIVOLA
Oswin Oettinger
Philipp Modlmeir
Blasius Hell
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Brembo SGL Carbon Ceramic Brakes GmbH
Original Assignee
SGL Carbon SE
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SGL Carbon SE filed Critical SGL Carbon SE
Publication of EP3687958A1 publication Critical patent/EP3687958A1/fr
Pending legal-status Critical Current

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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/571—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 from Si-containing polymer precursors or organosilicon monomers
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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
    • C04B35/52—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 carbon, e.g. graphite
    • C04B35/521—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 carbon, e.g. graphite obtained by impregnation of carbon products with a carbonisable material
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    • C04B35/52—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 carbon, e.g. graphite
    • C04B35/528—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 carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62625—Wet mixtures
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    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6269—Curing of mixtures
    • 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
    • F16D69/00—Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
    • F16D69/02—Composition of linings ; Methods of manufacturing
    • F16D69/023—Composite materials containing carbon and carbon fibres or fibres made of carbonizable material
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3826—Silicon carbides
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
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    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon
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    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C04B2235/6026—Computer aided shaping, e.g. rapid prototyping
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Definitions

  • the present invention relates to a ceramic component containing silicon carbide (SiC) and the use of the component.
  • Silicon carbide ceramics are generally characterized by their high hardness, good abrasion resistance, high chemical stability, high strength even at high temperatures
  • This ceramic is to compress carbonaceous fillers together with a binder and cure to a green body. The green body is then carbonized or pyrolyzed at elevated temperature to form a carbon body which is infiltrated with liquid silicon, the carbon reacting with silicon to form silicon carbide.
  • a composite containing, in addition to SiC, unreacted carbon, so-called free carbon, and free silicon.
  • a composite is referred to as a C / Si / SiC composite.
  • the terms "free silicon” and “free carbon” are understood to mean the elements in their pure form that are not chemically bound, or only with themselves, in such a composite material, the silicon carbide and the free carbon make inert components whereas free silicon is chemically and thermally the least stable component and can not withstand attacks from, for example, flux acids or hot alkalis such as hot NaOH or hot KOH as opposed to free carbon and silicon carbide
  • the operating temperature of the C / Si / SiC composite material is limited to a temperature that is less than the melting temperature of silicon, which is 1414 ° C.
  • the free carbon in such a composite material can indeed be attacked by oxidizing media
  • the carbon is by the liquid silicification with a SiC-Hül le encased and thus protected.
  • Components made of silicon carbide ceramic, which have a complex, geometric structure, are difficult to produce due to the high hardness of the ceramic by simple mechanical processing.
  • such components can be easily and inexpensively manufactured by means of an additive manufacturing process, the 3D printing process.
  • WO 2017/089494 A1 discloses ceramic composites containing SiC, which have also been produced using the 3D printing process.
  • a carbon molded body is produced by using a powder comprising coke and a liquid binder such as furan resin or phenolic resin. After the carbonization of the resulting carbon molded body, the silicization occurs.
  • the C / Si / SiC composites so produced typically have a free silicon content of greater than 30 weight percent (wt%) and a free carbon content of about 40 wt%.
  • These composite materials also show an inhomogeneous microstructure composition with comparatively large lakes or areas of free silicon and a proportion of free carbon which essentially derives from the carbon powder.
  • the chemical stability especially against acids or hot alkalis, such as, for example, hydrofluoric acid or hot NaOH liquor, and the temperature resistance of the ceramic composite materials containing silicon carbide are lowered ,
  • the object of the present invention is therefore to provide a ceramic component containing silicon carbide, which in addition to a high hardness, a high strength, a good abrasion resistance, also has a high chemical stability and a good temperature resistance.
  • this component should be able to be produced in practically unlimited geometric complexity easily and inexpensively.
  • this object is achieved by providing a ceramic component containing silicon carbide (SiC) obtainable by a process comprising the following steps:
  • a solution selected from the group consisting of a sugar solution, a starch solution or a cellulose solution, or a resin system comprising a mixture containing at least one resin, at least one solvent and at least one curing agent, wherein the at least one resin and that at least one solvent is different,
  • an above solution or a resin system comprising at least one resin, at least one solvent and at least one curing agent is used, wherein the at least one resin and the at least one solvent are different upon carbonization of the dried or hardened green body from the dried, fine-pored, foam-like solution or the hardened, sponge-like, fine-pored resin system, a fine-pored, foam-like or sponge-like carbon skeleton is formed (see FIG.
  • spongy carbon skeleton is used below, this term also stands for a foam-like carbon skeleton.
  • the pores of the green body are filled with silicon, whereby the pore volume of the sponge-like carbon skeleton is almost completely filled with silicon carbide.
  • the proportion of comparatively large lakes or areas of free silicon is markedly reduced compared to the prior art, as can be seen with reference to FIG.
  • the free silicon is thus no longer present in the form of large lakes or areas, but in these pores silicon carbide structures are present.
  • the presence of these silicon carbide structures which fill the pores results in higher chemical stability, greater hardness, and greater temperature resistance of the ceramic component.
  • Cisive in the use of a resin system for impregnating the green body is that the at least one resin and the at least one solvent are different. If the at least one resin and the at least one solvent are identical, carbonization of the cured green body based on carbon does not result in a fine-pored, sponge-like carbon skeleton, but instead in a compact resin carbon mold (see FIG. This results in the silicization that the carbonized resin carbon can be converted only superficially in SiC and a large part of the interior of the resin carbon due to the lack of accessibility for silicon is retained as carbon, whereby the SiC- comparatively content is only slightly increased.
  • the green body based on carbon in step a) is produced by means of a 3D printing process.
  • the production of such a green body can be carried out according to the methods described in WO 2017/089494.
  • a powdered composition having a grain size (d50) between 3 ⁇ and 500 ⁇ , preferably between 50 ⁇ and 350 ⁇ , more preferably between 100 ⁇ and 250 ⁇ comprising at least 50 wt .-% coke, preferably at least 80 wt. -%, more preferably at least 90 wt .-% and particularly preferably at least 95 wt .-% coke, and a liquid binder provided.
  • a planar deposition of a layer of the pulverulent composition followed by local deposition of droplets of the liquid binder on this layer.
  • the abovementioned pulverulent composition may be both a powder of primary particles and a granulate.
  • the term "d50" is understood to mean that 50% of the particles are smaller than the stated value The d50 value was determined with the aid of the laser granulometric method (ISO 13320) using a measuring device from Sympatec GmbH with associated evaluation software.
  • the following is to be understood as obtaining a green body having the desired shape of the component.
  • the green body Immediately after the curing or drying of the binder, the green body is still surrounded by a powder bed of loose particles of the powdered composition. The green body must therefore be removed from the powder bed or separated from the loose, non-solidified particles become.
  • This is referred to in the literature on 3D printing as "unpacking" of the printed component, which can be followed by a (fine) cleaning of the green body, in order to remove any adhering particle residues however, the type of unpacking is not particularly limited, and any known methods can be used.
  • the green body in step a) is coke, preferably selected from the group consisting of acetylene coke, flexikoks, fluid coke, petroleum coke, shot coke, coal tar. pitch coke, carbonized ion exchange bead coke, and any mixtures thereof, more preferably selected from the group consisting of acetylene coke, flexioks, fluid coke, shot coke, carbonized ion exchange bead coke, and any mixtures thereof.
  • the advantage of using these cokes is that they have a coke shape as round as possible, whereby the round shape leads to a good flowability and thus to a smooth 3D printing process.
  • Green coke is a coke, which still contains volatile constituents. These volatiles are almost no longer present in the calcined or carbonized coke, this coke undergoes a temperature treatment of typically 700 ° C to 1400 ° C.
  • the terms calcined or carbonized are understood as synonyms.
  • Graphitized coke is obtained by treating the coke at a temperature of normally more than 2000 ° C to 3000 ° C.
  • the coke may be admixed with a liquid activator, such as, for example, a liquid sulfuric acid activator.
  • a liquid activator such as, for example, a liquid sulfuric acid activator.
  • the use of such an activator can reduce the curing time and the necessary temperature for curing the binder, and on the other hand reduces the dust formation of the pulverulent composition.
  • the amount of activator is 0.05% to 3.0% by weight, more preferably 0.1% to 1.0% by weight, based on the total weight of coke and activator. If more than 3.0% by weight, based on the total weight of activator and coke, is used, the powdery composition sticks together and the flowability is reduced; be less than 0.05 wt .-% based on the
  • the selection of the binder for producing the 3D printed green body is not particularly limited. Suitable binders are, for example, phenolic resins, furan resins, polyimides, cellulose, starch, sugars, silicates, silicon-containing polymers, pitch, polyacrylonitrile (PAN) or any mixtures thereof. Also solutions of said binders are included herein. Basically, the binders should be such that after carbonation stable bodies can be obtained which survive handling when transferring to the siloing apparatus as well as the temperature used in the silicization.
  • the binder should have either a sufficiently high carbon yield or an Si-containing inorganic yield when using Si-organic binders after pyrolysis.
  • thermoplastic binders such as pitch
  • PAN The same applies to PAN.
  • the powder bed without binder additive acts as a support of the component, while the thermoplastic binder is carbonized as pitch or PAN.
  • the powder bed advantageously acts as oxidation protection for the printed green body during the subsequent carbonization treatment.
  • the binder phenolic resins, furan resins or polyimides are resins and polymers with a comparatively high carbon yield.
  • binders which are converted by curing into a non-fusible binder system and largely converted into SiC during siliciding. Due to their high carbon yield, most of the carbon is not converted to SiC during the siliconization process and carbon inclusions occur, resulting in an overall lighter component. Furthermore, the high carbon yield means that the content of free silicon in the component is correspondingly lower, resulting in improved chemical stability and higher temperature resistance.
  • cellulose, starch or sugar preferably in the present case as solution, can also be used as binder.
  • These binders only need to be dried, which is inexpensive, and the carbon residue resulting from the carbonation transforms ideally, that is, substantially completely, into SiC during the silicization.
  • silicates or silicon-containing polymers as binders, preferably present as a solution, has the advantage that these binders also only have to be cured. They form SiC when carbonated. Furthermore, wetting with liquid Si is better than with carbon, which facilitates the step of siliconization.
  • the fraction of the binder in the green body is preferably 1, 0 to 35.0% by weight, preferably 1.0 to 10.0% by weight and most preferably 1.5 to 5.0% by weight, based on the total weight of the green body.
  • the green body according to step a) contains not only carbon but also silicon carbide, preferably this green body contains up to 50% by weight of SiC based on the total weight of the green body.
  • the SiC used is used in the form of a powder, which preferably has a particle size (d50) between 50 and 500 ⁇ m, more preferably between 75 and 200 ⁇ m, having.
  • the laser granulometric method ISO 13320 was also used here, whereby a measuring device from Sympatec GmbH with associated evaluation software was used.
  • the oxidation stability of the ceramic component produced therewith is increased from the outset, since the proportion of free carbon in this component is reduced. Furthermore, this component has a high inertness to, for example, acids and alkalis, and the temperature resistance is maintained. Likewise, the hardness of the component is increased by the high final SiC content.
  • the above coke 3D printing method described above can be used, using a mixture of coke and silicon carbide instead of coke for the laydown step.
  • the impregnation of the green body according to step b) is carried out with a solution or a resin system.
  • the solution may be a sugar solution, preferably a monosaccharide, a polysaccharide or a mannitol solution, a starch solution or a cellulose solution.
  • a resin system for impregnating the green body in step b) it is preferable to use as the resin a phenol resin, a furan resin or any mixture of a phenolic resin with a furan resin.
  • the at least one solvent selected from the group consisting of water, a mono- or polyhydric alcohol, a mixture of at least two of the aforementioned alcohols, a mixture of water with at least one mono- and / or polyhydric alcohol or naphthalene.
  • monohydric alcohols for example, methanol, ethanol, propanols (n-propanol, iso-propanol) or butanols, for example n-butanol or sec-butanol, preferably ethanol, can be used; as polyhydric alcohols, for example, the dihydric alcohol glycol or the trihydric alcohol glycerol can be used.
  • the solvent in the curing step is entrapped in the resin system in the form of fine droplets of homogenous size, and then escapes in the carbonation step, leaving blank, i. unfilled, pores are formed, which provide a kind of sponge structure. Consequently, the pores also have a homogeneous size, which is advantageous in terms of the later homogeneous conversion of the amorphous carbon into silicon carbide.
  • the hardened resin system produces a fine-pored, sponge-like carbon skeleton.
  • the pores of the sponge-like carbon skeleton preferably have an average pore size of less than 50 ⁇ m, more preferably less than 20 ⁇ m, more preferably less than 10 ⁇ m and very particularly preferably less than 5 ⁇ m.
  • the mean pore size can be determined, for example, by a quantitative microstructure analysis in
  • the accessible surface of the carbon skeleton which is formed from the cured resin system, greatly increased, which ensures that the liquid silicon according to step e) can fill these pores for the most part completely.
  • the accessible surface of the carbon skeleton becomes larger the smaller the average pore size is. Since the carbon of said carbon skeleton with reacts quickly to the liquid silicon, this carbon can be largely converted into silicon carbide. At the same time, the original pores of the green body are largely filled by the sponge structure, which significantly reduces the lakes or areas of free silicon in the subsequent silicon infiltration.
  • the resin system which is used for impregnating the green body according to step b) preferably comprises as hardener an inorganic or organic acid, preferably an acid selected from the group consisting of dilute sulfuric acid, hydrochloric acid, phosphoric acid, boric acid, oxalic acid, maleic anhydride, Citric acid, malic acid, benzenesulfonic acids or phenolsulfonic acids, more preferably benzenesulfonic acids or phenolsulfonic acids, particularly preferably para-toluenesulfonic acid.
  • an inorganic or organic acid preferably an acid selected from the group consisting of dilute sulfuric acid, hydrochloric acid, phosphoric acid, boric acid, oxalic acid, maleic anhydride, Citric acid, malic acid, benzenesulfonic acids or phenolsulfonic acids, more preferably benzenesulfonic acids or phenolsulfonic acids, particularly preferably para-toluene
  • the at least one solvent is replaced by at least one propellant.
  • the at least one blowing agent is selected from the group consisting of halogenated hydrocarbons, preferably trichlorotrifluoroethane, pentanes, preferably, n-pentane, isopentane and cyclo-pentane, or stannous chloride.
  • the resin system for impregnating the green body according to step b) may also comprise a mixture of one of the above-mentioned hardeners and one of the said blowing agents.
  • at least one resin may be a two-component resin, preferably a polyurethane or an isocyanate resin.
  • the hardening of the impregnated green body in step c) can be carried out at room temperature or using a temperature which is lower than the boiling temperature of the solvent or the solvent mixture used, preferably the curing takes place at room temperature. Curing at room temperature is preferred since no application of temperature is necessary, which is a less expensive process step. This curing at room temperature is made possible because the resin system comprises a hardener. Furthermore, the
  • carbonizing is understood to mean the thermal conversion of the resin system containing the green body to carbon
  • the carbonization can be carried out by heating to temperatures in the range of 500 ° C.-1100 ° C., preferably 800 ° C up to 1000 ° C., under a protective gas atmosphere (eg under an argon or nitrogen atmosphere) with subsequent holding time
  • a protective gas atmosphere eg under an argon or nitrogen atmosphere
  • the siliconizing of the carbonized green body with liquid silicon in accordance with step e) can in principle take place under a protective gas atmosphere (eg Ar or He), in overpressure, normal pressure or in vacuo, preferably under reduced pressure.
  • a protective gas atmosphere eg Ar or He
  • overpressure normal pressure or in vacuo, preferably under reduced pressure.
  • the liquid silicon by itself, purely by means of capillary forces, can infiltrate the carbonized green body.
  • the present carbonized green bodies have exactly this desired property, ie that by means of the 3D printing process, the pore system of the carbonized green body can be designed such that without additional pressurization of the green body is completely infiltrated by capillary forces completely and virtually non-porous with silicon.
  • the silicization can be carried out in vacuo at a lower temperature, which of course must be above the melting temperature of silicon.
  • the above step e), ie the siliciding, is therefore preferably carried out under vacuum.
  • the liquid silicon designated in this context also comprises silicon alloys with a silicon content of at least 50% by weight in the context of the present invention. Preferably, however, pure silicon is used.
  • the siliciding, the green body to be silicided is preferably on
  • Wicks on which protrude from a bath from the silicon melt.
  • the wicks like the green body itself, are able to guide the liquid silicon through its porous structure by means of capillary forces.
  • the green body itself does not dip into the silicon bath but is located above it. After complete silicization and cooling to room temperature, the wick is connected to the component by the solidified silicon and must therefore be removed mechanically.
  • the wicks are preferably already provided as part of the green body, ie they are "printed" onto the green body by means of 3D printing during the production of the green body. with the wicks down, simply put in the container intended for the silicon bath. After completion of the silicidation and cooling, the wicks are mechanically removed as usual.
  • steps d) and e), ie the carbonization and the subsequent siliciding of the cured, impregnated green body take place virtually in a single process step, since during the siliconization the green body already carbonizes on heating the silicization temperature - so to speak in situ - with.
  • the steps of impregnating according to step b), drying or hardening according to step c) and carbonating according to step d) may be repeated at least once in said order, before the siliciding according to step e) is performed.
  • the pores of the green body framework are filled even more completely with the fine-pored spongy carbon framework which is formed by carbonating the dried solution or the hardened resin system.
  • the first impregnation is carried out with a resin system, and the second impregnation with a sugar, starch or cellulose solution. After the carbonization, the first impregnation step produces a fine-pored, sponge-like carbon skeleton which, however, does not completely fill the pores between the carbon grains.
  • the second impregnation step a sugar, starch or cellulose solution is used, which in the carbonation is a foam-like Carbon skeleton forms, the remaining pore spaces between the carbon grains are almost completely filled. This further increases the proportion of carbon which is converted into SiC during the subsequent siliconization and thus reduces the proportion of free silicon in the ceramic component. Furthermore, the density of the ceramic component is increased by this second impregnation step.
  • the lower content of free silicon increases the chemical resistance and the temperature resistance of the ceramic component, and the higher content of silicon carbide increases the hardness, rigidity and strength of the ceramic component.
  • Another aspect of this invention includes the method of making a ceramic component containing silicon carbide (SiC) as described in the application.
  • the ceramic component according to the invention which is based on a green body, in whose production no SiC powder, but exclusively carbon powder, was used, contains 20 to 60 wt .-%, preferably 30 to 50 wt .-%, SiC, 5 to 40 wt .-%, preferably 10 to 20 wt .-%, free silicon and 10 to 65 wt .-%, preferably 30 - 50 wt .-%, free carbon.
  • the proportion of free silicon, free carbon and silicon carbide was determined in the ceramic components according to DIN EN ISO 021068-2. The lower the proportion of free silicon, the higher the chemical stability and temperature resistance of the ceramic component. The proportion of free carbon plays a role in the oxidation resistance and stability of the ceramic component.
  • the ceramic component according to the invention which is based on a green body, in the production of which no SiC powder has been used, preferably has a breaking work of at least 200 Nmm, more preferably of at least 250 Nmm, particularly preferably of at least 300 Nmm. The fracture work was determined from the area of the bending deformation curve of the 3-point bending process.
  • the ceramic component according to the invention which is based on a green body, in the production of which no SiC powder was used, moreover preferably has a strength of at least 40 MPa, more preferably at least 60 MPa, more preferably at least 70 MPa, most preferably at least 80 MPa on.
  • This component is also sufficiently stable with respect to the mechanical stress.
  • the strength was determined according to the 3-point bending method according to DIN 51902.
  • the three-dimensional ceramic component according to the invention irrespective of whether SiC powder was used or not in the green body on which the component is based, is distinguished by its electrical conductivity, its high chemical and mechanical stability and hardness and its abrasion resistance.
  • Another aspect of the present invention is therefore the use of the inventive three-dimensional ceramic component as an impeller and separating or rotary valve in pumps and compressors, as pump housings, especially in the chemical industry, as internals in columns, as static mixer elements, as turbulators, as Burner nozzles, as burner inserts, as a lining of burner walls, as electrical contact, as electrical heating elements and supporting frames in high-temperature furnaces (especially because of the good thermal shock resistance) and as debuterlaufrad or reformerrad for mills for sifting mixtures of particles of different grain size.
  • this ceramic component according to the invention is characterized by good thermal conductivity and high chemical stability, high temperature resistance and high thermal shock resistance.
  • Yet another aspect of the present invention is therefore the use of the ceramic component according to the invention as a heat exchanger, as an element for heat exchangers, as a hot press matrix, as a heat sink in electronics, as a cooling housing for light emitting diodes or cameras or as a gauge.
  • this ceramic component according to the invention is characterized by its high mechanical hardness and abrasion resistance.
  • This makes it particularly suitable for use as a mechanically stressed component such as a slider in bearings or hinges comprising plain bearings and mechanical seals, a cam in gears, a gear, a sliding plate and a flexible tube, a piston and a piston sleeve, or machining tools in the form of milling cutters, drills, drill bits or indexable inserts.
  • Another aspect of the present invention is therefore the use of the ceramic component according to the invention as a mechanically stressed component comprising the above mechanically stressed components.
  • the ceramic component according to the invention also has a high abrasion resistance, it is suitable as a friction element for clutches and brakes.
  • Another aspect of the present invention is therefore also the use of the ceramic component according to the invention as a friction element for clutches and
  • Fig. 1 a shows a scanning electron micrograph (SEM image) of a carbonized green body based on carbon
  • Fig. 3 a shows a micrograph of a ceramic component based on carbon, which has been directly siliconized
  • FIG. 1 a shows an SEM image of a green body based on carbon, which has been produced by means of a 3D printing process.
  • carbonized binder ie, there are "carbonized binder bridges.”
  • the binder is the one used for the 3D printing process
  • furan resin (10 parts of furfuryl alcohol, 1 part of maleic anhydride)
  • the furfuryl alcohol functions as the resin and also functions as a viscosity-lowering solvent
  • Maleic anhydride acts as a hardener Carbonation, the resin system was cured at 160 ° C.
  • the carbonized resin rests on the walls of the pores of the carbon backbone. There may be large residual pores between the carbon grains.
  • the carbonized resin has not formed a fine-pored sponge-like carbon skeleton.
  • Green body based on carbon with a resin system comprising a
  • the carbonized green body has areas which constitute a fine-pored, sponge-like carbon skeleton. These areas are formed during carbonization from the cured resin system.
  • the microsection according to FIG. 3 a) shows a ceramic component based on
  • a calcined acetylene coke with a d50 of 190 ⁇ m was used. This was first mixed with 1, 0 wt .-% of a sulfuric acid liquid activator for phenolic resin, based on the total weight of coke and activator, and processed with a 3D-printing powder bed machine.
  • a Rackel unit placed on a flat powder bed a thin Kokspulverlage (about 0.3 mm in height) and a kind
  • Ink jet printing unit printed an alcoholic phenolic resin solution according to the desired component geometry on the coke bed. Subsequently, the printing table was lowered by the layer thickness and again applied a layer of coke and it was again printed phenolic resin locally. As a result of the repeated procedure, rectangular test specimens having, for example, the dimensions 120 mm (length) x 20 mm (width) x 20 mm (height) were constructed. Once the complete "component" had been printed, the powder bed was placed in a preheated to 140 ° C oven and held there for about 6 hours, the phenolic resin has hardened and formed a dimensionally stable green body.The excess coke powder was then sucked off after cooling and taken from the green body.
  • the carbon-based green body produced by a 3D printing method was subjected to vacuum impregnation with a mixture containing a resole resin (phenolic resin) having the trade name Norsophen 1203, water as a solvent and para-toluenesulfonic acid (dissolved in water) as a curing agent.
  • the hardener content in this mixture was 3.0% by weight.
  • the content of hardener in the above mixture is not greater than 10.0 wt.%, More preferably the content of hardener is between 1.0 and 6.0 wt.%, More preferably between 2.0 and 5.0 Wt .-%, in the above mixture.
  • the content of hardener in When this mixture is above 10.0% by weight, the formation of a fine-pored, sponge-like carbon skeleton does not occur during the carbonation of the cured resin system, and the pot life of the resin system for the impregnation treatment is too short. If the content of hardener in the above mixture is significantly less than 1.0% by weight, sufficient formation of a fine-pored sponge-like carbon skeleton does not take place, and the curing time becomes too long. On the other hand, if the content of the hardener in the above mixture is between 2.0 and 5.0% by weight, the content of the binder is good, and a fine-pored spongy carbon skeleton of the cured resin system after carbonization is formed. At the same time, the pot life of the resin is within a practicable range.
  • the silicon powder became liquid and rose by pure capillary action over the wicks in the 3D-printed, carbonized green body, without the additional gas or liquid pressure had to be applied. Large parts of the carbon reacted with the liquid silicon and formed silicon carbide. After cooling the furnace, the ceramic components were removed and the wicks removed mechanically. The resulting ceramic component had a free carbon content of 41% by weight, a free silicon content of 17% by weight, and a silicon carbide content of 42% by weight. The density of the obtained ceramic component was 2.4 g / cm 3 and was determined by the Archimedes method according to DIN 51918.
  • the carbon-based green body prepared by a 3D printing method was subjected to dip impregnation with a furan resin (10 parts of furfuryl alcohol, 1 part of maleic anhydride). After the step-shaped curing of the impregnated body using a temperature up to 160 °, the body was carbonized and siliconized analogously to the inventive example.
  • the obtained component had a free carbon content of 47% by weight, a free silicon content of 30% by weight, and a silicon carbide content of 23% by weight.
  • the density of the obtained ceramic component was 2.2 g / cm 3 and was determined by the Archimedes method.
  • Table 1 shows properties of the ceramic components containing silicon carbide prepared according to the non-inventive and the inventive example. The values listed here are averages.
  • the strength was determined according to the 3-point bending method according to DIN 51902.
  • the fracture energy was determined from the area of the bending deformation curve of the 3-point bending process. Elongation at break and stiffness (E-modulus) were also determined using the 3-point bending method mentioned above.
  • the universal hardness was determined according to DIN 50359-1. As the comparison of the examples shows, the strength, the stiffness (modulus of elasticity) and the fracture energy are higher in the case of the ceramic component according to the invention than in the case of the ceramic component according to the prior art.

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Abstract

L'invention concerne un composant céramique, le composant contenant de 20 à 60 % en poids de SiC, de 5 à 40 % en poids de silicium libre et de 10 à 65 % en poids de carbone libre, ainsi que l'utilisation du composant. Le procédé de réalisation comprend les étapes suivantes consistant à : a) fournir un corps cru à base de carbone qui a été produit par un procédé d'impression 3D; b) imprégner le corps cru avec une solution choisie dans le groupe comprenant une solution de sucre, une solution d'amidon et une solution de cellulose, ou avec un système de résine comprenant un mélange contenant au moins une résine, au moins un solvant et au moins un agent durcisseur, l'au moins une résine et l'au moins un solvant étant différents; c) sécher ou durcir le corps cru imprégné; d) carboniser le corps cru séché ou durci, un réseau carboné mousseux à pores fins étant formé à partir de la solution séchée ou un réseau carboné spongieux à pores fins étant formé à partir du système de résine durci; e) silicatiser le corps cru carbonisé par infiltration avec du silicium liquide.
EP18782380.2A 2017-09-28 2018-09-28 Composant céramique Pending EP3687958A1 (fr)

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DE102017217292.4A DE102017217292A1 (de) 2017-09-28 2017-09-28 Keramisches Bauteil
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DE102018208427B4 (de) * 2018-05-28 2022-03-17 Brembo Sgl Carbon Ceramic Brakes Gmbh Verfahren zur Herstellung eines Bauteils, das Bauteil selber und dessen Verwendung
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CA2380288A1 (fr) * 1999-07-23 2001-02-01 M Cubed Technologies, Inc. Composites de carbure de silicium et procedes de production correspondants
EP1359132A1 (fr) * 2002-04-30 2003-11-05 European Community Composites, applications, et leur procédé de fabrication
US20100015396A1 (en) * 2008-07-21 2010-01-21 General Electric Company Barrier coatings, methods of manufacture thereof and articles comprising the same
CN101811885B (zh) * 2010-05-05 2011-11-09 中国航空工业集团公司北京航空制造工程研究所 一种用呋喃树脂制备泡沫炭的方法
DE102011007815B4 (de) * 2011-04-20 2016-09-29 Sgl Carbon Se Verfahren zum Herstellen eines aus mehreren Vorkörpern zusammengefügten Keramikbauteils
CN102503430B (zh) * 2011-09-23 2013-10-16 中国科学院上海硅酸盐研究所 采用改进流延成型工艺制备反应烧结碳化硅陶瓷的方法
CN107249842A (zh) * 2014-08-27 2017-10-13 艾克斯温有限责任公司 通过三维打印制造碳制品的方法
JP6651754B2 (ja) * 2014-09-18 2020-02-19 Toto株式会社 反応焼結炭化ケイ素部材の製造方法
CN104496508B (zh) * 2014-12-01 2016-08-17 西安交通大学 基于光固化3D打印的SiC陶瓷基涡轮叶片的制造方法
DE102015223236A1 (de) * 2015-11-24 2017-05-24 Sgl Carbon Se Keramisches Bauteil
DE102015223240A1 (de) * 2015-11-24 2017-05-24 Sgl Carbon Se Kohlenstoff-Metall Verbundwerkstoff
CN106588060B (zh) * 2016-11-10 2019-08-20 中国科学院上海硅酸盐研究所 一种高致密的碳化硅陶瓷基复合材料及其制备方法

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CN111132951A (zh) 2020-05-08
US20200277234A1 (en) 2020-09-03

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