WO2013167518A2 - Céramique au nitrure de silicium et son procédé de fabrication - Google Patents

Céramique au nitrure de silicium et son procédé de fabrication Download PDF

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Publication number
WO2013167518A2
WO2013167518A2 PCT/EP2013/059357 EP2013059357W WO2013167518A2 WO 2013167518 A2 WO2013167518 A2 WO 2013167518A2 EP 2013059357 W EP2013059357 W EP 2013059357W WO 2013167518 A2 WO2013167518 A2 WO 2013167518A2
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WIPO (PCT)
Prior art keywords
silicon nitride
additive
nitride ceramic
sintering
ceramic
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PCT/EP2013/059357
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German (de)
English (en)
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WO2013167518A3 (fr
Inventor
Karl Berroth
Frank STEGNER
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Schaeffler Technologies AG & Co. KG
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Publication of WO2013167518A2 publication Critical patent/WO2013167518A2/fr
Publication of WO2013167518A3 publication Critical patent/WO2013167518A3/fr

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    • C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/76—Crystal structural characteristics, e.g. symmetry
    • C04B2235/767—Hexagonal symmetry, e.g. beta-Si3N4, beta-Sialon, alpha-SiC or hexa-ferrites
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/788—Aspect ratio of the grains
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Definitions

  • the present invention relates to a sintered silicon nitride ceramic, which in particular forms a component of a rolling or sliding bearing. Furthermore, the invention relates to a method for producing such
  • Silicon nitride ceramic Sintered silicon nitride ceramics are a frequently used material in mechanical and plant engineering, in the chemical industry, in foundry technology, in electronics, and because of their high strength, fracture toughness, wear, corrosion and thermal shock resistance as well as their low density and low thermal expansion in aerospace engineering.
  • EP 0 587 1 19 B1 shows a silicon nitride sintered body with a high content
  • Methods are 2.0% to 7.5% by weight of one or more
  • Rare earth elements in the form of the respective oxide as an additive added to the silicon nitride.
  • yttria and yttria are preferred embodiments.
  • Alumina is used as a single additive. In these embodiments, sintering takes place over a period of six hours at a temperature of 1,900 ° C.
  • a sintered body based on silicon nitride is known, which is intended for use in a rolling bearing. In the production of the sintered body, it is preferable to add 6% of yttrium oxide as an additive to the silicon nitride.
  • DE 602 18 549 T2 shows a roller bearing element with a silicon nitride
  • Sintered body which in addition to silicon nitride also 1 mass% to 10 mass%
  • Rolling element takes place after completion of the sintering preferably a Hot isostatic pressing treatment (HIP) in a non-oxidizing atmosphere of at least 300 atm (30 MPa) and at a temperature of 1,600 ° C to 1,880 ° C.
  • HIP Hot isostatic pressing treatment
  • Magnesium oxide powder can be used as additives for sintering.
  • the alumina powder and the alumina powder can be used as additives for sintering.
  • the alumina powder and the alumina powder can be used as additives for sintering.
  • Alumina powder and the magnesium oxide powder are for three to ten
  • DE 37 34 274 A1 shows an electrically insulating, ceramic sintered body, which preferably consists of a silicon nitride ceramic.
  • the spinel MgAI 2 O 4 is added as an additive.
  • DE 40 13 923 A1 shows a method for producing a silicon nitride powder, in which a spinel rare earth element oxide is preferably used as a sintering aid.
  • the spinel structure MgO ⁇ Al2O3 is used as a sintering additive.
  • the object of the present invention is a silicon nitride ceramic and a method for the production thereof
  • Silicon nitride ceramic which is designed in particular as a component of a rolling or sliding bearing, for example as a bearing ring or as a rolling element.
  • the method first comprises a step in which silicon nitride Si3N is provided.
  • the silicon nitride is preferably provided as a powder.
  • a first additive is provided as a sintering additive, which is a
  • the first additive is a perovskite-type chemical compound having a structure such as CaTiO 3. This structure is already present before a sintering process, so that the first additive can be described as presynthesized.
  • the first additive also acts as a sintering aid.
  • Process are the silicon nitride, the first additive and possibly further
  • Additives / additives mixed into a mixture.
  • the mixture is then formed into a green body, which is then sintered to a silicon nitride ceramic.
  • the sintering can be done for example by gas pressure sintering or by a hot pressing process.
  • Perovskits a particularly homogeneous distribution of liquid phase sintering necessary elements in the Si3N ceramic is achieved. This results in a particularly advantageous sintering behavior, which it u. a. allows to dispense with a hot isostatic sintering compaction of Si3N ceramic. Instead, it is possible
  • a particular advantage of the method according to the invention is also that oxidic compounds / elements can be used as sintering additives during the production process, which have hygroscopic properties in intrinsic form (eg La 2 O 3 , Nd 2 O 3 , P ⁇ Os) and themselves therefore
  • the first additive to be used according to the invention in the form of a presensitized perovskite does not prove to be hygroscopic, but is also stable in an aqueous environment.
  • the mixing of the silicon nitride powder and the at least first additive and the further treatment can therefore also be carried out on an aqueous basis, so that it is possible to dispense with a much more expensive and dangerous solvent-based preparation.
  • a drying of the ground mixture is preferably carried out to a fine, free-flowing granules.
  • Granules to the green body is preferably carried out by pressing into a mold.
  • the first additive has the following general chemical formula:
  • RE is at least one
  • Rare earth metal while M stands for at least one metal. Furthermore, 0.4 ⁇ x ⁇ 1, 6.
  • x 1, so that there is a stoichiometrically balanced chemical compound REMO3.
  • x ⁇ 1 more preferably x ⁇ 0.8.
  • x> 1 particularly preferably x> 1, 2.
  • Perovskitstrukur is modified if necessary, so that at least one perovskite-like structure is present, which is within the scope of the invention.
  • the component M is preferably selected from the group formed by Al, Fe, Cr and Mn, wherein the component M may comprise one or more of these metals. Particularly preferably, the component M comprises at least aluminum Al.
  • the component RE particularly preferably comprises at least neodymium Nd.
  • the first additive has the formula NdxAl 2-x O 3 , which is a concretization of the abovementioned general chemical formula.
  • the first additive has the formula NdAIO3, which is a
  • the additive has the following general chemical formula:
  • RE 1 stands for a first rare earth metal
  • the first additive is preferably provided in the form of particles which have an average primary particle size of less than 1 ⁇ m. These are therefore nanoscale primary particles, which are preferably formed as nanoparticles are.
  • the phar particles can also be present in particular as granules or agglomerates.
  • the average primary particle size of the first additive is preferably from about 10 nm to several 100 nm
  • the primary particle size of the first additive is preferably less than 500 nm.
  • the average primary particle size of the first additive is preferably more than 50 nm.
  • the proportion of the first additive is preferably between 10% by weight and 30% by weight of the mixture.
  • the proportion of the first additive is preferably between 10 wt .-% and 15 wt .-%, more preferably between 12 wt .-% and 13.5 wt .-% of the mixture. Basically, a share of more than
  • the proportion of the silicon nitride is preferably between 60 wt .-% and 95 wt .-%, more preferably between
  • no further additive of the mixture is added in addition to the first additive.
  • Silicon nitride only the first additive only the first additive.
  • the exclusive use of the The first additive as an additive ensures that the first additive is extremely homogeneously distributed in the mixture.
  • Method is provided in addition to the first additive, a second additive and added to the mixture.
  • the second additive is preferably in the form of primary particles, which have an average primary particle size of less than 1 ⁇ .
  • the second additive is preferably such chemical
  • this second additive is preferably selected from the group of oxides and nitrides of the elements Ti, Hf, Zr, Mo, Ta, Nb and Cr and the oxides and nitrides of the rare earth metals.
  • the second additive may comprise several of the compounds mentioned.
  • the proportion of the second additive is preferably at most 5 wt .-% of the mixture.
  • a third additive is provided and added to the mixture.
  • the third additive can be added both when using the first and second additive as well as when using the first additive alone.
  • the third additive is preferably present in the form of primary particles, which an average
  • Primary particle size of less than 1 ⁇ have.
  • the third additive is preferably such chemical
  • the third additive is preferably MgO, Al 2 O 3, Y 2 O 3 or AlN.
  • the third additive is preferred by a spinel or by a garnet educated.
  • the third additive may comprise several of said compounds.
  • the proportion of the third additive is preferably at most 5 wt .-% of the
  • the sintering is carried out at a temperature between 1 .500 ° C and 2,000 ° C, more preferably between 1 .700 ° C and 1 .900 ° C. In alternative preferred embodiments, the sintering is carried out at a temperature of between 1, 700 ° C and 2000 ° C.
  • the duration of sintering is preferably between one minute and 60 minutes, more preferably between 20 minutes and 30 minutes. In alternative preferred embodiments, the duration for sintering is between one hour and four hours, more preferably between two hours and three hours.
  • the provision of the particles of the first additive preferably takes place in that the substance of the first additive is precipitated from a liquid phase.
  • the provision of the particles of the first additive preferably takes place in that a
  • Primary particle size and a specific surface can be achieved by the subsequent grinding of coarser particles.
  • the sintering of the green body is preferably carried out by sintering
  • the silicon nitride ceramic produced according to the invention is already densely sintered to a large extent without pores and has high-quality microstructures and properties, preference is given to none
  • Hot isostatic pressing performed.
  • An advantage of the method according to the invention is that no or only a thin sintered skin of the silicon nitride ceramic is formed. The while sintering
  • resulting sintered skin has a thickness which is preferably less than 0.5 mm, more preferably less than 0.2 mm and more preferably less than 0.1 mm.
  • Silicon nitride ceramic is also preferably no measure is taken to reduce the oxygen content in the edge region of the silicon nitride ceramic, such as, for example, a deoxidation treatment before sintering.
  • a further object of the invention is a silicon nitride ceramic, which is obtainable by the method according to the invention.
  • a further subject of the invention is a silicon nitride ceramic which is sintered and, in addition to silicon nitride, comprises a grain boundary phase which is formed by a chemical compound of silicon nitride and a first additive having a perovskite structure.
  • the silicon nitride is preferably crystallized in the form of ⁇ -Si3N-stalk crystals.
  • the grain boundary phase is preferably formed in a glass-like manner between the ⁇ -Si 3 N stalk crystals.
  • the grain boundary phase preferably has the general chemical formula RE a Si b McO d N e , in which RE is a rare earth metal and M is a metal, where a, b, c, d and e are greater than zero.
  • the silicon nitride ceramic according to the invention has in terms of their
  • composition in particular with regard to the chemical composition of the bound in the grain boundary phase first additive and optionally further
  • the average particle size of the first additive preferably less than 1 ⁇ , more preferably less than 500 nm. Further for example, the average particle size of the first additive is more than 50 nm.
  • bonded first additive is preferably similar to the chemical composition of the first additive, which is preferably used according to the inventive method.
  • the chemical composition of any other additives present in the sintered silicon nitride ceramic is preferably the same
  • the silicon nitride ceramic according to the invention is characterized in that it has a high strength and at the same time good fracture toughness. So is the
  • 3-point bending strength of the silicon nitride ceramic according to the invention preferably at least 800 MPa, more preferably more than 900 MPa.
  • the crack toughness according to Niihara is at the same time at least 6 MPa "0.5 , preferably more than 7 MPa " 0.5 , particularly preferably about 7.5 to 8.7 MPa "0.5
  • the compressive strength of the silicon nitride ceramic according to the invention is preferably at least 2500 MPa, more preferably more than 3,000 MPa.
  • the silicon nitride ceramic according to the invention preferably has a morphology with predominantly acicular ⁇ -Si 3 N crystals, which are present in the glassy or
  • the needle-shaped crystals ensure a high fracture toughness and damage tolerance of the
  • the needle-shaped crystals have a large relative length. Accordingly, the acicular crystals have a length and a diameter whose ratio is on average preferably greater than 4, more preferably greater than 8.
  • at least one-tenth of the needle-shaped crystals of the silicon nitride ceramic according to the invention has a length and a
  • Diameter the ratio is greater than 10, more preferably greater than 20.
  • the silicon nitride ceramic according to the invention is preferably formed without pores, without being subjected to a hot isostatic pressing or a comparable
  • Preferred embodiments of the silicon nitride ceramic according to the invention have a sintered skin which is less than 0.5 mm, more preferably less than 0.2 mm and more preferably less than 0.1 mm thick, without the sintering skin being reduced by a measure after sintering ,
  • the silicon nitride ceramic according to the invention is preferably designed as a component of a bearing, for example as a component of a sliding bearing or a roller bearing.
  • Silicon nitride ceramic according to the invention at least comprises, also one
  • the component of the bearing is formed by the silicon nitride ceramic according to the invention.
  • the silicon nitride ceramic according to the invention is preferably designed as a bearing ring or as a rolling element.
  • Fig. 1 a micrograph of a preferred embodiment of a
  • FIG. 3 shows a micrograph of the silicon nitride ceramic according to the invention in a higher resolution
  • FIG. 4 shows a micrograph of the silicon nitride ceramic according to the prior art in a higher resolution; a micrograph of a cross-sectional area of the edge region of the preferred embodiment of the invention
  • Silicon nitride ceramic according to the prior art.
  • Silicon nitride powder prepared in aqueous medium with the addition of appropriate additives, such as a condenser and a defoamer.
  • Fluidized bed granulation The granules produced were then processed by the molding processes of a cold isostatic pressing (CIP) or a uniaxial dry pressing with cold isostatic densification into green bodies and if necessary in terms of geometry, dimensional accuracy, tolerance and surface quality by machining processes, such as drilling, turning, milling, grinding, etc. reworked as close to final contour as possible in the green state. Subsequently, a thermal debinding step was carried out to remove all the organic components which are disadvantageous for the subsequent sintering but which are necessary for shaping.
  • CIP cold isostatic pressing
  • a uniaxial dry pressing with cold isostatic densification into green bodies and if necessary in terms of geometry, dimensional accuracy, tolerance and surface quality by machining processes, such as drilling, turning, milling, grinding, etc. reworked as close to final contour as possible in the green state.
  • a thermal debinding step was carried out to remove all the organic components which are disadvantageous for the subsequent sintering but
  • the sintering of the moldings was then carried out depending on the type of sintering additive used and sintering additive content at temperatures between 1 .700 ° C and 1 .900 ° C in a gas pressure sintering furnace under non-oxidizing atmosphere with temporary application of a gas pressure of 0.5 MPa to 10 MPa.
  • the density of the ceramic was determined by comparing the samples or the determined by the measurement method according to Archimedes component density and the
  • Helium pycnometry measured on a very pulverulent material sample determined true density of the silicon nitride material determined. From the produced ceramic samples or components were subsequently
  • Test specimen for the determination of the 3- or 4-point bending strength according to DIN EN 843-1 worked out and subjected to the measurement.
  • the determination of the modulus of elasticity was carried out by evaluating the stress-strain ratio from the 3- or 4-point bending test according to the standard DIN EN 843-2,
  • the hardness test was carried out by Vickers HV20 hardness impressions according to the DIN EN 843-4 standard on finely polished material ground sections.
  • the fracture toughness test was carried out by measuring the cracks coming from the corners of the hardness impressions and calculating according to the formula for the fracture toughness K
  • the statistical evaluation of all determined mechanical characteristics was carried out according to the DIN EN 843-5 standard issued for monolithic ceramics.
  • one RExAl 2-x O 3 was used as the first additive, where RE is a rare earth metal and 0.4 ⁇ x ⁇ 1, 6.
  • This is a perovskite structure, which in the context of the invention is stoichiometric in the case of x 1 (see Table 1),
  • Table 1 shows various proportions of rare earth oxides REO and
  • Alumina AI2O3 for the inventive provision of various proportions of the first additive, each having a stoichiometric composition for the
  • Table 2 shows various proportions of rare earth oxides REO and
  • the data in Table 2 are in% by weight.
  • Table 3 shows various proportions of rare earth oxides REO and
  • Alumina AI2O3 for the provision according to the invention of various proportions of the first additive, each having a substoichiometric composition (x 0.8) for gas pressure sintering.
  • the data in Table 3 are in% by weight.
  • Table 4 shows various concentrations of the elements Nd, Al and O as well as concentrations of neodymium oxide and alumina for the invention particularly preferred provision of NdAIO3 as the first additive for gas pressure sintering.
  • the data in Table 4 are in% by weight.
  • Fig. 1 shows a micrograph of a preferred embodiment of a
  • silicon nitride ceramic of the present invention (Example No. 6 in Table 5) prepared by the addition of a first additive having a perovskite structure and can be described by the formula NdxAl 2-x O3 with 0.4 ⁇ x ⁇ 1.6.
  • This chemical compound NdxAl 2-x O3 did not first form during sintering, but was added in this form as an additive to the silicon nitride before sintering. It is thus a presynthesized additive.
  • the silicon nitride ceramic shown is approximately free of pores and homogeneously sintered.
  • the very few, black dots, however, indicate small residual pores 01 in the material.
  • the white microstructure constituents in the polished section are due to the introduction of a third additive as coloring agent, which forms crystallized grains 02 having a size of 1 ⁇ m to 2 ⁇ m.
  • FIG. 2 shows a prior art silicon nitride ceramic which has been subjected to hot isostatic pressing (HIP) with about 12% by weight of sintering additive content, so that it has a comparatively high compressive strength of more than
  • HIP hot isostatic pressing
  • the silicon nitride ceramic according to the invention shown in FIG. 1 was not subjected to a hot isostatic pressing process, so that it was produced much less laboriously and yet has a comparable structure to the silicon nitride ceramic produced in accordance with the prior art shown in FIG. 2.
  • Silicon nitride ceramics also have a compressive strength of about 3,000 MPa, and also the fracture toughness reaches approximately the same at 6.9 MPa "0.5
  • the prior art silicon nitride ceramic shown in Fig. 2 also has a dyeing additive included in the silicon nitride ceramic in the form of crystallized grains 03, which are recognizable as white dots.
  • the grains 03 have a size of about 1 ⁇ to 2 ⁇ on. Despite sintering and densification by hot isostatic pressing (HIP) are also in the Microstructure of this silicon nitride ceramic fine residual pores 04 with approximately similar frequency and size as in Fig. 1 recognizable.
  • HIP hot isostatic pressing
  • Fig. 3 shows a further microsection of the preferred embodiment of
  • Silicon nitride ceramic according to the invention in a higher resolution.
  • the micrograph shows a scale of 10 ⁇ .
  • the silicon nitride ceramic has a morphology with acicular ⁇ -Si 3 N crystals 06 which are present in the structure in a three-dimensional and statistically oriented manner, resulting in a quasi-isotropic microstructure and the quasi-isotropic properties of the ceramic.
  • the needle-shaped crystals are surrounded by the glassy or semi-crystalline grain boundary and filling phase formed from the first and optionally third additive and the SiO 2 fraction of the starting Si 3 N powder.
  • Filling phase is formed by a chemical compound of silicon nitride and the first additive having a perovskite structure.
  • Crystals 06 have a length and a diameter whose ratio is in many cases more than 10 and occasionally up to 24.
  • the needle-shaped crystals 06 cause a high fracture toughness and thus damage tolerance of
  • FIG. 4 shows a further micrograph of the prior art silicon nitride ceramic shown in FIG. 2 in a higher resolution. It is the same resolution as in Fig. 3, to the invention shown in Fig. 3
  • Silicon nitride ceramic to compare with the prior art.
  • the silicon nitride ceramic according to the prior art shown in FIG. 4 predominantly has only short acicular ⁇ -Si 3 N crystals 07, so that in contrast to
  • Silicon nitride ceramic according to the invention only a significantly reduced
  • Silicon nitride ceramic has no or only a very thin sinter skin on its surface 08, without having to remove or reduce a sinter skin for this purpose by means of a hard-machining step.
  • FIG. 6 shows, in comparison to FIG. 5, a cross-sectional area of a silicon nitride ceramic according to the prior art. This silicon nitride ceramic has on its surface on a sintered skin 09, which must be removed for many applications by a subsequent hard machining, but significantly increases the manufacturing cost.
  • Table 6 shows various proportions of rare earth oxides REO and
  • Alumina AI2O3 for the inventive provision of various proportions of the first additive, each having a stoichiometric composition (x 1, 0) for hot pressing.
  • the data in Table 6 are in% by weight.
  • Table 7 shows various proportions of rare earth oxides REO and
  • Alumina AI2O3 for the provision according to the invention of various proportions of the first additive, each having a superstoichiometric composition (x 1, 2) for hot pressing.
  • the data in Table 7 are in wt .-%.
  • Table 8 shows various proportions of rare earth oxides REO and
  • Alumina AI2O3 for the provision according to the invention of various proportions of the first additive, each having a substoichiometric composition (x 0.8) for hot pressing.
  • the data in Table 8 are in% by weight.
  • Table 9 shows various concentrations of the elements Nd, Al and O as well as concentrations of neodymium oxide and alumina to the invention particularly preferred provision of NdAIO3 as the first additive for hot pressing.
  • the data in Table 9 are in wt .-%.
  • Table 9 Representative examples Nos. 8 to 11 for the property values of the ceramic materials hot-pressed according to the present invention are shown in Table 10.

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Abstract

La présente invention concerne une céramique au nitrure de silicium frittée, qui constitue en particulier un composant d'un palier à roulement ou d'un palier lisse. L'invention concerne en outre un procédé de fabrication d'une telle céramique au nitrure de silicium. Ce procédé comporte une première étape consistant à préparer du nitrure de silicium Si3N4. Le procédé consiste ensuite à préparer un premier additif présentant une structure pérovskite. Ce premier additif est un composé chimique du type perovskite qui présente une structure telle que CaTiO3. Cette structure est déjà présente avant un processus de frittage, de sorte que le premier additif peut être qualifié de présynthétisé. Le premier additif sert par ailleurs d'agent de frittage. Une autre étape du procédé selon l'invention consiste à mélanger le nitrure de silicium et le premier additif pour obtenir un mélange. Ce mélange est ensuite façonné pour produire un comprimé cru qui est alors fritté pour produire une céramique au nitrure de silicium.
PCT/EP2013/059357 2012-05-10 2013-05-06 Céramique au nitrure de silicium et son procédé de fabrication WO2013167518A2 (fr)

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