WO2014187643A1 - Produit en graphite et son procédé de fabrication - Google Patents

Produit en graphite et son procédé de fabrication Download PDF

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Publication number
WO2014187643A1
WO2014187643A1 PCT/EP2014/058393 EP2014058393W WO2014187643A1 WO 2014187643 A1 WO2014187643 A1 WO 2014187643A1 EP 2014058393 W EP2014058393 W EP 2014058393W WO 2014187643 A1 WO2014187643 A1 WO 2014187643A1
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WO
WIPO (PCT)
Prior art keywords
graphite
thermal expansion
form factor
product
coefficient
Prior art date
Application number
PCT/EP2014/058393
Other languages
German (de)
English (en)
Inventor
Helge Jansen
Christos Aneziris
Petra Stein
Original Assignee
Refratechnik Holding Gmbh
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 Refratechnik Holding Gmbh filed Critical Refratechnik Holding Gmbh
Priority to EP14723352.2A priority Critical patent/EP2999678A1/fr
Publication of WO2014187643A1 publication Critical patent/WO2014187643A1/fr

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Classifications

    • 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
    • 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
    • C04B35/52—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
    • C04B35/522—Graphite
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5292—Flakes, platelets or plates
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • 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
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • 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
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • 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
    • C04B2235/5463—Particle size distributions
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • 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
    • C04B2235/5463—Particle size distributions
    • C04B2235/5472—Bimodal, multi-modal or multi-fraction
    • 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
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/785—Submicron sized grains, i.e. from 0,1 to 1 micron
    • 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
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron
    • 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
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Definitions

  • the invention relates to a molded product made of graphite (graphite product), in particular a refractory shaped graphite product and a process for its preparation.
  • Graphite has a hexagonal structure and consists of a sequence of different layers, the so-called graphene layers, which propagate in an ab plane and are superimposed in the c direction and are held together only by weak Van der Waals interactions.
  • the density of graphite varies greatly depending on the origin and degree of comminution. Due to the layer structure, some properties of graphite are strongly direction-dependent, such as electrical conductivity, thermal conductivity and mechanical properties.
  • a particular disadvantage of graphite is its low oxidation resistance. It increases with increasing crystallinity of the carbon material.
  • Refractory molded graphite products are e.g. B. usually in large blocks or shaped stones for z. As furnace linings or as molds or crucibles or as wells and electrodes for the production of aluminum.
  • the raw material is usually calcined natural graphite, which in coarse crystalline platelet form as so-called Flake graphite with carbon contents between 86 and 99, in particular between 92 and 98% and particle sizes z. B. between> 200 and ⁇ 500 microns is used.
  • Natural graphite available on the market comes mainly from deposits in China, Brazil, Norway, Canada, India and North Korea.
  • As a binder for the graphite is in the production of graphite blocks or graphite bricks z. B.
  • coke scaffold the spatial shape of the blocks or stones.
  • the natural graphites available on the market which are suitable for refractory products, differ in terms of storage due in particular also in the dimensions in the flakes, resulting in differences in mechanical properties.
  • synthetic graphites are also on the market.
  • This object is achieved by a homogeneous graphite mixture of at least two with respect to a particle size parameter different Graphitsorten from particular natural occurrence, the reversible thermal expansion of the graphite mixture and the resulting graphite product from the difference of the reversible thermal expansion of the two graphites, z.
  • the at least two graphite locations are selected on the basis of a respective form factor FF, which has previously been determined for the respective graphite species.
  • the thermal expansion coefficient ⁇ is meant, which characterizes the reversible thermal expansion. Not meant is an irreversible stretching and irreversible shrinkage, but the elongation with temperature increase, which goes back equally with temperature lowering.
  • the determined maximum or average grain size or other specific grain sizes of a graphite cake are not suitable for correlating with the reversible thermal expansion so that the reversible thermal expansion of the mixture is not without a mixture of at least two graphite species of different particle sizes Another is controllable. It has been shown that not every finely divided or coarser graphite grade alike influences the reversible thermal expansion of another graphite species, because the reversible thermal expansion of the graphite does not correlate exclusively with its fineness.
  • a determinable form factor of a graphite cake correlates with its reversible thermal expansion.
  • the form factor is calculated from a determined grain size determined by a sieve analysis and an average calculated from an optical measurement of the thickness of a plurality of flakes of the flake graphite species. The number of flakes to be measured results z. B. from statistical Specifications that the expert knows and z. B. the standard ASTM E1 12 are shown.
  • the form factor FF is thus calculated from the following formula:
  • the sieve For example, for a first graphite cake by sieving the sieve is determined in which 90 wt .-% of the graphite cake pass through the sieve (d 90 value). This d 90 value gives z. B. a grain size of 200 pm.
  • the average thickness c (the average) is determined by measuring the thickness of a plurality of flakes, with z. B. 10 microns. This results in the following value for the form factor FF of this first graphite with
  • the difference between two form factors in a graphite cake mixture is expediently at least 10, in particular at least 50, preferably at least 80.
  • the blended amount of the other graphite, the additional graphite depends on the level of the desired reduction of the reversible thermal expansion of the graphite to be changed, which is without significant influence on other properties of the respective, containing a certain amount of graphite refractory product, in which according to the invention now a graphite mixture is included, which has a reduced reversible thermal expansion corresponding to the Rajgraphitsortenmenge.
  • the added amount of attorneygraphitsorte is z. B.
  • FIG. 1 shows a scanning electron micrograph (SEM image) of a rock graphite variety available on the market with details of a few optically measured flake thicknesses;
  • Fig. 2 is a graphical illustration of the correlation between the coefficient of thermal expansion and the shape factor of various types of graphite in the respective d 90 value.
  • the reversible thermal expansion or the coefficient of thermal expansion of a graphite powder is z. B. determined by a cold isostatic pressed graphite test specimen is prepared and then the thermal expansion is measured.
  • a mixture of the graphite with a novolak powder resin plus resin hardener z For example, hexamethylenetetramine, from 95 Ma.% Graphite and 5 Ma.% Resin including 10 Ma.% Hardener, based on the resin.
  • the graphite cylinder is placed in a measuring capsule which is filled with petroleum coke for protection against burning off of the carbon, and for the measurement of the thermal expansion a hood furnace z. B. the company Netzsch used.
  • the prepared measuring capsule is installed in the hood furnace and has a load of 0.02 MPa applied and the specimen heated to 1500 ° C.
  • the thermal expansion is determined with a recorded strain curve.
  • the calculation of the thermal expansion coefficient ⁇ then takes place from the increase in the expansion curve as a function of the temperature, determined on the basis of DIN-EN 993-19.
  • the SEM image ( Figure 1) shows several graphite flakes of a marketed flake graphite variety, some of which are labeled "GF".
  • the optical analog ASTM E 112 is given a certain thickness, the measured location being a
  • a mixture of 80% by weight of the first flake graphite and 20% by weight of the second flake weight graphite cake gave a CTE of 10.2 ⁇ 10 -6 K -1 .
  • a mixture of 90% by weight of the first flake graphite and 10% by weight of the second flake graphite yielded a CTE of 11.9 ⁇ 10 -6 K -1.
  • a mixture of 70% by weight of the first flake graphite and 30% by weight. % of the second flake graphite yielded a CTE of 8.5 x 10 -6 K -1 .
  • Fig. 2 shows the correlation of the coefficient of thermal expansion of various flake graphite varieties to the shape factor of the graphite species, the values being on a slightly bent connecting line. ones shown, is the correlation with d 90 values of the flake graphites.
  • correlation lines arise with other d x values up to z. D 50 values or x values above 90. The higher this pass value, the more accurate the correlation.
  • the d x value should therefore advantageously be between d 50 and d 95 .
  • the same x x value for the flake graphites to be analyzed eg., to select the d 90 value for the available flake graphite varieties and, based on the calculated shape factor, the additional graphite or additional graphite grades with which the coefficient of thermal expansion of a graphite mainly used can be clearly controlled by admixing an additional graphite species.
  • Desirable is a screening according to ASTM E11-87 or ISO 565.
  • the inventive method for controlling the reversible thermal expansion is effectively applicable to pure graphite products, especially pure refractory graphite products, which consist mainly of graphite, such as crucibles, graphite blocks and other graphite components, because inventive mixing of at least two different Flockengraphitsorten, z. B. originating from different deposits, flake graphite can be produced with significantly changed reversible thermal expansion. This makes z. B. sense, if you only want to change the reversible thermal expansion of a graphite and the other original properties of the graphite product to be preserved.
  • d x value from a screening to evaluate at least one SEM image of a flake graphite by the graph length a and the graphene width b of a statistically sufficient number of flakes optically, z.
  • ASTM E112 the averaged thickness c of the graphite flakes of this graphite variety, which is likewise determined and also from the same SEM image.
  • the product has a homogeneous mixture of at least two grades of graphite, each with different coefficients of thermal expansion, with one graphite cake predominating in quantity and the other type of graphite acts as a supplementary graphite, (claim 1)
  • Graphite differs in a form factor FF, which correlates with its coefficient of thermal expansion
  • the form factor FF results in each case by a division of a Siebmaschenweite in microns, through which a certain percentage graphite flake x of graphite passes through this (d x value), by a at least one SEM image optically determined and computationally averaged thickness c of visible on the SEM image flakes of graphite, wherein a small form factor FF with a high coefficient of thermal expansion and a larger form factor FF with a smaller coefficient of thermal expansion correlates ⁇ claim 2)
  • the form factor FF of suitable natural graphite grades is between 5 and 200, in particular between 10 and 100, (claim 3) x of the d x value is between 50 and 95, in particular between 60 and 90, preferably 90, (claim 4)
  • the difference of the shape factors FF ( ⁇ FF) of the graphite varieties of the graphite cake mixture is at least 10, in particular at least 50 and preferably at least 85. (Claim 5)
  • a particularly advantageous method for reducing the reversible thermal expansion of a shaped graphite product, in particular of natural graphite, in particular a refractory shaped graphite product, is when a mixture of graphite and at least one binder is prepared and molded and solidified, wherein graphite is a mixture of at least two graphite grades is used, which differ with their thermal expansion coefficient, in particular a graphite species quantitatively predominates and the other graphite serves as Rajgraphitsorte (claim 7), wherein it is advantageous if
  • the graphite varieties differ in a shape factor FF correlated with their thermal expansion coefficient, one graphite species having a lower form factor FF and making up the predominant constituent of the graphite mixture and the other graphite having a higher form factor FF or vice versa, depending on which coefficient of thermal expansion is to be changed , and wherein the shape factor FF of each graphite is determined before mixing, (claim 8)
  • each form factor FF is determined as follows:
  • Graphites with form factors FF of at least 10, in particular of at least 50 and preferably at least 100 are used for the production of graphite mixtures, (claim 10)
  • the mesh size is determined using x-values between 50 and 95, in particular between 60 and 90, preferably 90, (claim 1 1)
  • Graphitsorten be used for a graphite mixture whose difference between their form factors FF ( ⁇ FF) at least is at least 3 and at most 50 and in particular between 5 and 30, (claim 12)
  • the additional amount of graphite with the larger form factor FF to the graphite with the smaller form factor FF or vice versa, depending on which coefficient of thermal expansion is to be changed, is at least 3 and at most 50 wt .-% and in particular between 5 and 30 wt .-%. (Claim 13)

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

L'invention concerne un produit en graphite façonné, en particulier réfractaire, composé de graphite, en particulier de graphite naturel, qui est solidifié par un liant connu en soi pour former un corps façonné, le produit comprenant essentiellement un mélange homogène d'au moins deux types de graphite présentant chacun des coefficients de dilatation thermique différents, un type de graphite étant quantitativement prépondérant et l'autre type de graphite faisant office de type de graphite additionnel. L'invention concerne également un procédé de fabrication du produit en graphite.
PCT/EP2014/058393 2013-05-23 2014-04-24 Produit en graphite et son procédé de fabrication WO2014187643A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP14723352.2A EP2999678A1 (fr) 2013-05-23 2014-04-24 Produit en graphite et son procédé de fabrication

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102013008856.9A DE102013008856B4 (de) 2013-05-23 2013-05-23 Graphiterzeugnis und Verfahren zu seiner Herstellung
DE102013008856.9 2013-05-23

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WO2014187643A1 true WO2014187643A1 (fr) 2014-11-27

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Application Number Title Priority Date Filing Date
PCT/EP2014/058393 WO2014187643A1 (fr) 2013-05-23 2014-04-24 Produit en graphite et son procédé de fabrication

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Country Link
EP (1) EP2999678A1 (fr)
DE (1) DE102013008856B4 (fr)
WO (1) WO2014187643A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116952305A (zh) * 2023-07-31 2023-10-27 江苏宏基高新材料股份有限公司 一种等静压石墨机加工检验系统

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2035984A (en) * 1978-12-05 1980-06-25 Toshin Steel Co Graphite refractory article having dense structure with low porosity
FR2542309A1 (fr) * 1983-03-12 1984-09-14 Kurosaki Refractories Co Materiaux refractaires contenant du graphite
WO2011125536A1 (fr) * 2010-03-31 2011-10-13 黒崎播磨株式会社 Matériau réfractaire contenant du graphite lamellaire à structure grossière

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3948000B2 (ja) * 2003-08-26 2007-07-25 松下電器産業株式会社 高熱伝導性部材及びその製造方法ならびにそれを用いた放熱システム
US20090057940A1 (en) * 2007-09-04 2009-03-05 Aruna Zhamu Method of producing less anisotropic flexible graphite

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2035984A (en) * 1978-12-05 1980-06-25 Toshin Steel Co Graphite refractory article having dense structure with low porosity
FR2542309A1 (fr) * 1983-03-12 1984-09-14 Kurosaki Refractories Co Materiaux refractaires contenant du graphite
WO2011125536A1 (fr) * 2010-03-31 2011-10-13 黒崎播磨株式会社 Matériau réfractaire contenant du graphite lamellaire à structure grossière

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP2999678A1 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116952305A (zh) * 2023-07-31 2023-10-27 江苏宏基高新材料股份有限公司 一种等静压石墨机加工检验系统
CN116952305B (zh) * 2023-07-31 2024-05-17 江苏宏基高新材料股份有限公司 一种等静压石墨机加工检验系统

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DE102013008856B4 (de) 2016-09-29
EP2999678A1 (fr) 2016-03-30
DE102013008856A1 (de) 2014-11-27

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