WO2022049818A1 - Refractory material - Google Patents

Refractory material Download PDF

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Publication number
WO2022049818A1
WO2022049818A1 PCT/JP2021/014378 JP2021014378W WO2022049818A1 WO 2022049818 A1 WO2022049818 A1 WO 2022049818A1 JP 2021014378 W JP2021014378 W JP 2021014378W WO 2022049818 A1 WO2022049818 A1 WO 2022049818A1
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Prior art keywords
refractory material
less
sic particles
sic
particle size
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PCT/JP2021/014378
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French (fr)
Japanese (ja)
Inventor
常夫 古宮山
浩臣 松葉
裕樹 臼杵
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日本碍子株式会社
エヌジーケイ・アドレック株式会社
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Application filed by 日本碍子株式会社, エヌジーケイ・アドレック株式会社 filed Critical 日本碍子株式会社
Priority to CN202180004708.2A priority Critical patent/CN115956064A/en
Priority to JP2021568109A priority patent/JP7167367B2/en
Priority to KR1020227002200A priority patent/KR20220033050A/en
Publication of WO2022049818A1 publication Critical patent/WO2022049818A1/en

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    • 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
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
    • 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
    • C04B35/56—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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/14—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment
    • F27B9/20—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace
    • F27B9/24—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace being carried by a conveyor
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/14—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment
    • F27B9/20—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace
    • F27B9/24—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace being carried by a conveyor
    • F27B9/2407—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace being carried by a conveyor the conveyor being constituted by rollers (roller hearth furnace)
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/30—Details, accessories, or equipment peculiar to furnaces of these types
    • F27B9/36—Arrangements of heating devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D3/00—Charging; Discharging; Manipulation of charge
    • F27D3/12—Travelling or movable supports or containers for the charge
    • 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
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon
    • 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

Definitions

  • Patent Document 1 discloses a technique relating to a Si—SiC refractory material (silicon / silicon carbide composite material).
  • the refractory material of Patent Document 1 is composed of SiC particles having an average particle size of 0.01 to 2 ⁇ m, SiC particles having an average particle size of 0.1 to 10 ⁇ m, and metallic Si dispersed among the SiC particles.
  • Si-SiC material Si impregnated SiC
  • metallic Si is dispersed between SiC particles which are aggregates, and the toughness and mechanical strength of the refractory material are improved.
  • the refractory material disclosed in the present specification may be a SiC material in which SiC particles are mainly used as an aggregate and metallic Si is contained between the SiC particles. Further, the average particle diameter of the SiC particles as the aggregate is 10 ⁇ m or less, and when the cross section of the refractory material is observed, 100 or more pores of 0.05 ⁇ m or more and 25 ⁇ m or less exist in the range of 100 ⁇ m ⁇ 100 ⁇ m. It's okay.
  • the refractory material can form a roller, a setter for firing, and a beam for a heating furnace.
  • An example (roller) of a refractory material is shown.
  • An example of a refractory material (firing setter) is shown. It is an example of a refractory material (beam for a heating furnace), (a) shows the appearance of a beam for a heating furnace, and (b) shows a cross section of a beam for a heating furnace. The results of the examples are shown.
  • the refractory material disclosed in the present specification can be used as a component of a heating furnace or a part used in the heating furnace. Specifically, it can be used as a wall material of a heating furnace, a beam (beam), a roller of a continuous heating furnace, a setter for firing for mounting an object to be fired (object to be fired), and the like.
  • the refractory material may be a SiC-SiC refractory material in which SiC particles are mainly used as the aggregate and metallic Si is contained between the SiC particles.
  • SiC particles having excellent heat resistance as the main component of the aggregate
  • the heat resistance of the refractory material can be improved.
  • "mainly SiC particles as the aggregate” means that the ratio of the SiC particles to the total mass of the aggregate is 50% by mass or more. That is, the aggregate constituting the refractory material may contain particles other than SiC particles.
  • the ratio of SiC particles to the aggregate may be 60% by mass or more, 70% by mass or more, 80% by mass or more, or 90% by mass or more. However, it may be 95% by mass or more.
  • the refractory material may contain, for example, B4 C particles and C particles in addition to the SiC particles as the aggregate.
  • the average particle size of the SiC particles may be 15 ⁇ m or less.
  • the average particle size of the aggregate (SiC particles) may be 10 ⁇ m or less, 7 ⁇ m or less, 5 ⁇ m or less, 3 ⁇ m or less, or 1 ⁇ m or less. good.
  • the minimum particle size of the aggregate may be 0.05 ⁇ m or more.
  • the particle size (average particle size, minimum particle size, maximum particle size) of the SiC particles can be confirmed by observing the cross section of the fireproof material using a scanning electron microscope (SEM) or the like.
  • the refractory material may have 100 or more pores of 0.05 ⁇ m or more and 25 ⁇ m or less in the range of the cross section of the refractory material of 100 ⁇ m ⁇ 100 ⁇ m.
  • small-sized pores pores of 0.05 ⁇ m or more and 25 ⁇ m or less
  • the size of the pores can be confirmed by observing the cross section of the refractory material using a scanning microscope or the like, similarly to the particle size of the aggregate. Specifically, the size of the pores can be confirmed by observing a range of the cross section of the refractory material of 100 ⁇ 100 ⁇ m and measuring the maximum diameter of the pores appearing in the range.
  • the porosity (apparent porosity) of the refractory material may be 1% or less. This improves the mechanical strength of the refractory material.
  • the porosity (apparent porosity) of the refractory material may be 0.8% or less, 0.6% or less, and 0.5% or less.
  • the porosity of the refractory material can be measured in accordance with JIS R2205-1992.
  • the refractory material disclosed in the present specification contains metallic Si between SiC particles.
  • the ratio of metallic Si to the refractory material may be 20% by mass or more and 60% by mass or less.
  • the proportion of metallic Si in the refractory material may be 55% by mass or less, 50% by mass or less, 45% by mass or less, 40% by mass or less, and 35% by mass. It may be less than or equal to%.
  • the ratio of the metallic Si to the refractory material is 20% by mass or more, the metallic Si can sufficiently fill the gaps between the SiC particles (the increase in the apparent porosity is suppressed).
  • the ratio of metallic Si to the refractory material may be 30% by mass or more, and may be 40% by mass or more.
  • FIG. 1 shows a roller 10 used in a heating furnace (not shown).
  • the roller 10 has a cylindrical shape having a through hole 12, and is made of a Si—SiC material.
  • the roller 10 is an example of a refractory material.
  • the roller 10 is composed of SiC particles having a particle size of 0.4 to 15 ⁇ m and an average particle diameter of 30 ⁇ m as an aggregate. Further, metallic Si is present between the SiC particles.
  • the particle size of the aggregate (SiC particles) was calculated by acquiring an SEM image of the cross section of the central portion of the roller 10 and measuring the shape of the aggregate existing in the range of 100 ⁇ m ⁇ 100 ⁇ m in the image.
  • the aggregate (SiC particles) and the substance (metal Si) between the aggregates were identified by performing elemental analysis on the acquired SEM image using EDS.
  • the porosity (apparent porosity) of the roller 10 was 0.5%. As a result of performing a bending strength test on the roller 10 in accordance with JIS R1601-2008, it was 448 MPa.
  • the roller 10 was manufactured by an extrusion molding method. Since the extrusion molding method is known, the description thereof will be omitted.
  • FIG. 2 shows a setter 14 used in a heating furnace (not shown).
  • the setter 14 has the same characteristics as the roller 10.
  • the setter 14 can be manufactured by a pressing method.
  • FIG. 3 shows a beam 16 constituting a heating furnace (not shown). As shown in (a) and (b), the beam 16 is columnar and solid. The beam 16 can be manufactured by an extrusion molding method.
  • FIG. 4 shows the particle size of the aggregate used when preparing each sample.
  • a cylindrical (roller-shaped) molded body having an outer diameter of 38 mm, an inner diameter of 25 mm, and a length of 1000 mm is produced by an extrusion molding machine.
  • the temperature was 100 ° C., and the mixture was dried in an air atmosphere for 24 hours or more.
  • After impregnating with metallic Si it was fired at 1600 ° C. in an inert gas (Ar) atmosphere to obtain a Si—SiC-quality roller-shaped refractory material.
  • FIG. 4 shows the measurement results of the bending strength.
  • " ⁇ " is given to the sample having a bending strength of 350 MPa or more
  • " ⁇ ” is given to the sample having a bending strength of 300 MPa or more and less than 350 MPa
  • " ⁇ " is shown for the sample having a bending strength of 200 MPa or more and less than 300 MPa.
  • Samples less than or equal to are marked with an "x”.
  • " ⁇ " and " ⁇ " are pass levels.
  • the particle size of the SiC particles (average particle size, minimum particle size, maximum particle size), the number of pores in the cross-sectional observation in the range of 100 ⁇ m ⁇ 100 ⁇ m, the porosity, the formability, and the retention.
  • the shape was also evaluated.
  • the particle size of the SiC particles was calculated by observing the cross section of the refractory material by SEM and measuring all the SiC particles appearing within the range of 100 ⁇ m ⁇ 100 ⁇ m.
  • the cross section of the refractory material was observed by SEM, and the pores within the range of 100 ⁇ m ⁇ 100 ⁇ m (pores of 0.05 ⁇ m or more and 25 ⁇ m or less) were visually counted.
  • the porosity (apparent porosity) was measured in accordance with JIS R2205-1992.
  • the cross-sectional SEM observation was performed using TM4000 manufactured by Hitachi High-Technologies Corporation. The results of the number of pores and the porosity are shown in FIG.
  • the sample after extrusion molding is visually observed, and the sample in which no abnormality is confirmed is marked with " ⁇ ", the sample in which deformation is confirmed is marked with " ⁇ ”, and the sample in which deformation and breakage (sheet breakage) are confirmed.
  • the sample was evaluated as “ ⁇ ”, and the sample that could not be molded due to frequent sheet breakage during extrusion was evaluated as "x”.
  • samples (samples 1 to 6) having an average particle size of SiC particles of 15 ⁇ m or less and having 100 or more pores of 0.05 ⁇ m or more and 25 ⁇ m or less have good strength (300 MPa or more).
  • particularly good strength (350 MPa or more) can be obtained for the samples (samples 1 to 5) having the maximum particle diameter of the SiC particles of 30 ⁇ m or less.
  • the samples (Samples 1 to 3) having a maximum particle size of SiC particles of 15 ⁇ m or less can obtain extremely good strength (400 MPa or more).
  • the samples (Samples 1 to 6) showing good strength all had a minimum particle size of 0.05 ⁇ m or more and an apparent porosity of 1% or less. It was confirmed that Samples 1 to 6 had better moldability and shape retention than Samples 7 to 9.
  • samples 1 to 3 can obtain extremely high-strength refractory materials. Comparing Samples 1 to 3 and Samples 4 to 6, Samples 1 to 3 have a feature that the apparent porosity is 0.5% or less. From this result, it was confirmed that the strength of the refractory material can be further improved by setting the apparent porosity of the refractory material to 0.5% or less.
  • a roller, a setter, and a beam using a refractory material have been shown, but the refractory material disclosed in the present specification is a part other than the above-mentioned embodiment as long as it is a part used in a high temperature environment. It can also be used as a product).
  • a columnar beam is shown, but the beam may be a prismatic beam.
  • roller 14 Firing setter 16: Beam for heating furnace

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Abstract

This refractory material is a Si-SiC material with SiC particles as the main aggregate and metallic Si contained between the SiC particles. Furthermore, the average particle size of the SiC particles, which are the aggregate, is 15 μm or less, and when the cross section of the refractory material is observed, 100 or more pores in the range of 0.05-25 μm are present in the range of 100 × 100 μm.

Description

耐火材Refractory material
　本出願は、２０２０年９月７日に出願された日本国特許出願第２０２０－１５００６０号に基づく優先権を主張する。その出願の全ての内容は、この明細書中に参照により援用されている。本明細書は、耐火材に関する技術を開示する。特に、ＳｉＣ粒子間に金属Ｓｉが含まれるＳｉ－ＳｉＣ質の耐火材に関する技術を開示する。 This application claims priority based on Japanese Patent Application No. 2020-150060 filed on September 7, 2020. The entire contents of that application are incorporated herein by reference. This specification discloses techniques relating to refractory materials. In particular, a technique relating to a SiC-SiC refractory material containing metallic Si between SiC particles is disclosed.
　特開２００４－１８３３２号公報（以下、特許文献１と称する）に、Ｓｉ－ＳｉＣ質の耐火材（シリコン／炭化ケイ素複合材料）に関する技術が開示されている。特許文献１の耐火材は、平均粒径が０．０１～２μｍのＳｉＣ粒子と、平均粒径が０．１～１０μｍのＳｉＣ粒子と、ＳｉＣ粒子間に分散した金属Ｓｉによって構成されている。 Japanese Unexamined Patent Publication No. 2004-18332 (hereinafter referred to as Patent Document 1) discloses a technique relating to a Si—SiC refractory material (silicon / silicon carbide composite material). The refractory material of Patent Document 1 is composed of SiC particles having an average particle size of 0.01 to 2 μm, SiC particles having an average particle size of 0.1 to 10 μm, and metallic Si dispersed among the SiC particles.
　Ｓｉ－ＳｉＣ質（Ｓｉ含浸ＳｉＣ）は、骨材であるＳｉＣ粒子間に金属Ｓｉが分散しており、耐火材の靭性及び機械的強度等の特性が向上する。しかしながら、耐火材の薄肉化、あるいは、高耐久化（長寿命化）のため、さらなる特性の向上が必要とされている。本明細書は、Ｓｉ－ＳｉＣ質の耐火材において、高強度の耐火材を提供することを目的とする。 In the Si-SiC material (Si impregnated SiC), metallic Si is dispersed between SiC particles which are aggregates, and the toughness and mechanical strength of the refractory material are improved. However, in order to make the refractory material thinner or to have higher durability (longer life), it is necessary to further improve the characteristics. It is an object of the present specification to provide a high-strength refractory material in a Si—SiC refractory material.
　本明細書で開示する耐火材は、骨材としてＳｉＣ粒子を主体とし、そのＳｉＣ粒子間に金属Ｓｉが含まれるＳｉ－ＳｉＣ質であってよい。また、骨材であるＳｉＣ粒子の平均粒子径が１０μｍ以下であり、耐火材の断面を観察したときに、０．０５μｍ以上２５μｍ以下の気孔が、１００μｍ×１００μｍの範囲に１００個以上存在していてよい。なお、この耐火材は、ローラー、焼成用セッター、加熱炉用ビームを形成することができる。 The refractory material disclosed in the present specification may be a SiC material in which SiC particles are mainly used as an aggregate and metallic Si is contained between the SiC particles. Further, the average particle diameter of the SiC particles as the aggregate is 10 μm or less, and when the cross section of the refractory material is observed, 100 or more pores of 0.05 μm or more and 25 μm or less exist in the range of 100 μm × 100 μm. It's okay. The refractory material can form a roller, a setter for firing, and a beam for a heating furnace.
耐火材の一例（ローラー）を示す。An example (roller) of a refractory material is shown. 耐火材の一例（焼成用セッター）を示す。An example of a refractory material (firing setter) is shown. 耐火材の一例（加熱炉用ビーム）であり、（ａ）は加熱炉用ビームの外観を示し、（ｂ）は加熱炉用ビームの断面を示す。It is an example of a refractory material (beam for a heating furnace), (a) shows the appearance of a beam for a heating furnace, and (b) shows a cross section of a beam for a heating furnace. 実施例の結果を示す。The results of the examples are shown.
　本明細書で開示する耐火材は、加熱炉の構成部品、あるいは、加熱炉内で用いられる部品として利用することができる。具体的には、加熱炉の壁材、ビーム（梁）、連続式加熱炉のローラー、被焼成物（被加熱物）を載置するための焼成用セッター等として利用することができる。 The refractory material disclosed in the present specification can be used as a component of a heating furnace or a part used in the heating furnace. Specifically, it can be used as a wall material of a heating furnace, a beam (beam), a roller of a continuous heating furnace, a setter for firing for mounting an object to be fired (object to be fired), and the like.
　耐火材は、骨材としてＳｉＣ粒子を主体とし、ＳｉＣ粒子間に金属Ｓｉが含まれるＳｉ－ＳｉＣ質の耐火材であってよい。耐熱性に優れたＳｉＣ粒子を骨材の主体とすることにより、耐火材の耐熱性を向上させることができる。なお、「骨材としてＳｉＣ粒子を主体とする」とは、骨材の全質量に占めるＳｉＣ粒子の割合が５０質量％以上であることを意味している。すなわち、耐火材を構成する骨材は、ＳｉＣ粒子以外の粒子を含んでいてもよい。なお、骨材に占めるＳｉＣ粒子の割合は、６０質量％以上であってよいし、７０質量％以上であってよいし、８０質量％以上であってよいし、９０質量％以上であってよいし、９５質量％以上であってもよい。なお、耐火材は、骨材としてＳｉＣ粒子に加え、例えば、Ｂ４Ｃ粒子、Ｃ粒子を含んでいてもよい。 The refractory material may be a SiC-SiC refractory material in which SiC particles are mainly used as the aggregate and metallic Si is contained between the SiC particles. By using SiC particles having excellent heat resistance as the main component of the aggregate, the heat resistance of the refractory material can be improved. In addition, "mainly SiC particles as the aggregate" means that the ratio of the SiC particles to the total mass of the aggregate is 50% by mass or more. That is, the aggregate constituting the refractory material may contain particles other than SiC particles. The ratio of SiC particles to the aggregate may be 60% by mass or more, 70% by mass or more, 80% by mass or more, or 90% by mass or more. However, it may be 95% by mass or more. The refractory material may contain, for example, B4 C particles and C particles in addition to the SiC particles as the aggregate.
　ＳｉＣ粒子の平均粒子径は、１５μｍ以下であってよい。これにより、耐火材の構造（組織構造）が緻密化し、耐火材の機械的強度を向上させることができる。骨材（ＳｉＣ粒子）の平均粒子径は、１０μｍ以下であってよいし、７μｍ以下であってよいし、５μｍ以下であってよいし、３μｍ以下であってよいし、１μｍ以下であってもよい。なお、骨材の最小粒子径は、０．０５μｍ以上であってよい。耐火材を製造する際、骨材（粒子）が凝集することを抑制することができる。また、骨材の最大粒子径は、１５μｍ以下であってよい。耐火材の組織構造内において骨材自体が欠陥となることが抑制され、耐火材の機械的強度の低下を抑制することができる。ＳｉＣ粒子の粒径（平均粒子径、最小粒子径、最大粒子径）は、走査型顕微鏡（ＳＥＭ）等を利用し、耐火材の断面観察によって確認することができる。 The average particle size of the SiC particles may be 15 μm or less. As a result, the structure (structural structure) of the refractory material can be refined and the mechanical strength of the refractory material can be improved. The average particle size of the aggregate (SiC particles) may be 10 μm or less, 7 μm or less, 5 μm or less, 3 μm or less, or 1 μm or less. good. The minimum particle size of the aggregate may be 0.05 μm or more. When producing a refractory material, it is possible to suppress the aggregation of aggregates (particles). The maximum particle size of the aggregate may be 15 μm or less. It is possible to prevent the aggregate itself from becoming a defect in the tissue structure of the refractory material, and it is possible to suppress a decrease in the mechanical strength of the refractory material. The particle size (average particle size, minimum particle size, maximum particle size) of the SiC particles can be confirmed by observing the cross section of the fireproof material using a scanning electron microscope (SEM) or the like.
　耐火材は、耐火材の断面１００μｍ×１００μｍの範囲に、０．０５μｍ以上２５μｍ以下の気孔が１００個以上存在していてよい。換言すると、小サイズの気孔（０．０５μｍ以上２５μｍ以下の気孔）が、耐火材の内部に分散して存在していてよい。耐火材の内部に大サイズの気孔（例えば５０μｍ超の気孔）が存在することを抑制でき、耐火材の機械的強度を向上させることができる。すなわち、破壊の起点となり得る大サイズの気孔が耐火材の内部に存在することを抑制することにより、耐火材の機械的強度が向上する。なお、気孔の大きさは、骨材の粒径と同様に、走査型顕微鏡等を利用し、耐火材の断面観察によって確認することができる。具体的には、気孔の大きさは、耐火材の断面１００×１００μｍの範囲を観察し、その範囲に現れる気孔の最大径を測定することにより確認することができる。 The refractory material may have 100 or more pores of 0.05 μm or more and 25 μm or less in the range of the cross section of the refractory material of 100 μm × 100 μm. In other words, small-sized pores (pores of 0.05 μm or more and 25 μm or less) may be dispersed inside the refractory material. It is possible to suppress the existence of large-sized pores (for example, pores having a size of more than 50 μm) inside the refractory material, and it is possible to improve the mechanical strength of the refractory material. That is, the mechanical strength of the refractory material is improved by suppressing the existence of large-sized pores that can be the starting point of fracture inside the refractory material. The size of the pores can be confirmed by observing the cross section of the refractory material using a scanning microscope or the like, similarly to the particle size of the aggregate. Specifically, the size of the pores can be confirmed by observing a range of the cross section of the refractory material of 100 × 100 μm and measuring the maximum diameter of the pores appearing in the range.
　また、耐火材の気孔率（見掛け気孔率）は、１％以下であってよい。これにより、耐火材の機械的強度が向上する。耐火材の気孔率（見掛け気孔率）は、０．８％以下であってよく、０．６％以下であってよく、０．５％以下であってよい。なお、耐火材の気孔率は、ＪＩＳ　Ｒ２２０５－１９９２に準拠して測定することができる。 Further, the porosity (apparent porosity) of the refractory material may be 1% or less. This improves the mechanical strength of the refractory material. The porosity (apparent porosity) of the refractory material may be 0.8% or less, 0.6% or less, and 0.5% or less. The porosity of the refractory material can be measured in accordance with JIS R2205-1992.
　上記したように、本明細書で開示する耐火材は、ＳｉＣ粒子間に金属Ｓｉが含まれている。耐火材に占める金属Ｓｉの割合は、２０質量％以上、６０質量％以下であってよい。耐火材に占める金属Ｓｉの割合が６０質量％以下であれば、耐火材の製造過程（主として焼成工程）において、内部クラックの発生を抑制することができる。なお、耐火材に占める金属Ｓｉの割合は、５５質量％以下であってよく、５０質量％以下であってよく、４５質量％以下であってよく、４０質量％以下であってよく、３５質量％以下であってもよい。また、耐火材に占める金属Ｓｉの割合が２０質量％以上であれば、金属ＳｉがＳｉＣ粒子間の隙間を十分に充填することができる（見掛け気孔率が増大することが抑制される）。耐火材に占める金属Ｓｉの割合は、３０質量％以上であってよく、４０質量％以上であってもよい。 As described above, the refractory material disclosed in the present specification contains metallic Si between SiC particles. The ratio of metallic Si to the refractory material may be 20% by mass or more and 60% by mass or less. When the ratio of metallic Si to the refractory material is 60% by mass or less, the generation of internal cracks can be suppressed in the process of manufacturing the refractory material (mainly the firing step). The proportion of metallic Si in the refractory material may be 55% by mass or less, 50% by mass or less, 45% by mass or less, 40% by mass or less, and 35% by mass. It may be less than or equal to%. Further, when the ratio of the metallic Si to the refractory material is 20% by mass or more, the metallic Si can sufficiently fill the gaps between the SiC particles (the increase in the apparent porosity is suppressed). The ratio of metallic Si to the refractory material may be 30% by mass or more, and may be 40% by mass or more.
　図１は、加熱炉（図示省略）で用いられるローラー１０を示している。ローラー１０は、貫通孔１２を有する円筒状であり、Ｓｉ－ＳｉＣ質で形成されている。ローラー１０は、耐火材の一例である。ローラー１０は、骨材として、粒径０．４～１５μｍ、平均粒子径３０μｍのＳｉＣ粒子で構成されている。また、ＳｉＣ粒子間には、金属Ｓｉが存在している。なお、骨材（ＳｉＣ粒子）の粒径は、ローラー１０の中央部分の断面のＳＥＭ画像を取得し、画像内の１００μｍ×１００μｍの範囲に存在する骨材の形状を測定し、算出した。また、骨材（ＳｉＣ粒子）及び骨材間の物質（金属Ｓｉ）は、取得したＳＥＭ画像についてＥＤＳを用いて元素分析を行うことにより特定した。 FIG. 1 shows a roller 10 used in a heating furnace (not shown). The roller 10 has a cylindrical shape having a through hole 12, and is made of a Si—SiC material. The roller 10 is an example of a refractory material. The roller 10 is composed of SiC particles having a particle size of 0.4 to 15 μm and an average particle diameter of 30 μm as an aggregate. Further, metallic Si is present between the SiC particles. The particle size of the aggregate (SiC particles) was calculated by acquiring an SEM image of the cross section of the central portion of the roller 10 and measuring the shape of the aggregate existing in the range of 100 μm × 100 μm in the image. In addition, the aggregate (SiC particles) and the substance (metal Si) between the aggregates were identified by performing elemental analysis on the acquired SEM image using EDS.
　取得したＳＥＭ画像の１００μｍ×１００μｍの範囲には、０．０５μｍ以上２５μｍ以下の気孔が７２２個確認され、１５μｍ超の気孔は確認されなかった。ローラー１０の気孔率（見掛け気孔率）は、０．５％であった。ローラー１０について、ＪＩＳ　Ｒ１６０１－２００８に準拠して曲げ強度試験を行った結果、４４８ＭＰａであった。なお、ローラー１０は、押出成型法により作製した。押出成形法については、公知のため、説明を省略する。 In the range of 100 μm × 100 μm of the acquired SEM image, 722 pores of 0.05 μm or more and 25 μm or less were confirmed, and no pores of more than 15 μm were confirmed. The porosity (apparent porosity) of the roller 10 was 0.5%. As a result of performing a bending strength test on the roller 10 in accordance with JIS R1601-2008, it was 448 MPa. The roller 10 was manufactured by an extrusion molding method. Since the extrusion molding method is known, the description thereof will be omitted.
　図２は、加熱炉（図示省略）で用いられるセッター１４を示している。セッター１４は、ローラー１０と同様の特性を有している。セッター１４は、プレス法により作製することができる。 FIG. 2 shows a setter 14 used in a heating furnace (not shown). The setter 14 has the same characteristics as the roller 10. The setter 14 can be manufactured by a pressing method.
　図３は、加熱炉（図示省略）を構成するビーム１６を示している。（ａ）及び（ｂ）に示すように、ビーム１６は円柱状であり、中実である。ビーム１６は、押出成型法により作製することができる。 FIG. 3 shows a beam 16 constituting a heating furnace (not shown). As shown in (a) and (b), the beam 16 is columnar and solid. The beam 16 can be manufactured by an extrusion molding method.
　骨材（ＳｉＣ粒子）の粒径（平均粒子径）が異なる耐火材（試料１～９）を作製し、曲げ強度の測定を行った。図４に、各試料を作製する際に用いた骨材の粒径を示す。具体的な耐火物の作成方法としては、まず、図４に示す骨材を用い、押出成形機にて外径３８ｍｍ、内径２５ｍｍ、長さ１０００ｍｍの円筒状（ローラー状）の成形体を作製し、温度１００℃、大気雰囲気下で２４時間以上乾燥させた。その後、金属Ｓｉを含浸させた後、不活性ガス（Ａｒ）雰囲気下で１６００℃にて焼成し、Ｓｉ－ＳｉＣ質のローラー状耐火材を得た。 Fireproof materials (samples 1 to 9) having different particle sizes (average particle size) of aggregates (SiC particles) were prepared, and bending strength was measured. FIG. 4 shows the particle size of the aggregate used when preparing each sample. As a specific method for producing a refractory material, first, using the aggregate shown in FIG. 4, a cylindrical (roller-shaped) molded body having an outer diameter of 38 mm, an inner diameter of 25 mm, and a length of 1000 mm is produced by an extrusion molding machine. , The temperature was 100 ° C., and the mixture was dried in an air atmosphere for 24 hours or more. Then, after impregnating with metallic Si, it was fired at 1600 ° C. in an inert gas (Ar) atmosphere to obtain a Si—SiC-quality roller-shaped refractory material.
　得られた試料１～９について曲げ強度の測定を行った。曲げ強度は、ＪＩＳ　Ｒ１６０１－２００８に準拠して測定した。図４に、曲げ強度の測定結果を示す。なお、図４には、曲げ強度の測定結果と併せ、曲げ強度が３５０ＭＰａ以上の試料に「◎」、３００ＭＰａ以上３５０ＭＰａ未満の試料に「〇」、２００ＭＰａ以上３００ＭＰａ未満の試料に「△」、２００ＭＰａ未満の試料に「×」を付して示している。「◎」及び「〇」が合格レベルである。また、試料１～９について、曲げ強度の他、ＳｉＣ粒子の粒径（平均粒子径、最小粒子径、最大粒子径）、１００μｍ×１００μｍ範囲の断面観察における気孔数、気孔率、成形性、保形性の評価も行った。 The bending strength was measured for the obtained samples 1 to 9. The bending strength was measured according to JIS R1601-2008. FIG. 4 shows the measurement results of the bending strength. In addition, in FIG. 4, together with the measurement result of the bending strength, "◎" is given to the sample having a bending strength of 350 MPa or more, "○" is given to the sample having a bending strength of 300 MPa or more and less than 350 MPa, and "Δ" is shown for the sample having a bending strength of 200 MPa or more and less than 300 MPa. Samples less than or equal to are marked with an "x". "◎" and "○" are pass levels. Further, for the samples 1 to 9, in addition to the bending strength, the particle size of the SiC particles (average particle size, minimum particle size, maximum particle size), the number of pores in the cross-sectional observation in the range of 100 μm × 100 μm, the porosity, the formability, and the retention. The shape was also evaluated.
　ＳｉＣ粒子の粒径（平均粒子径、最小粒子径、最大粒子径）は、耐火材の断面をＳＥＭ観察し、１００μｍ×１００μｍ範囲内に現れたＳｉＣ粒子を全てについて測定し、算出した。気孔数は、耐火材の断面をＳＥＭ観察し、１００μｍ×１００μｍ範囲内の気孔（０．０５μｍ以上２５μｍ以下の気孔）を目視でカウントした。また、気孔率（見掛け気孔率）は、ＪＩＳ　Ｒ２２０５－１９９２に準拠して測定した。なお、断面のＳＥＭ観察は、（株）日立ハイテクノロジーズ社製のＴＭ４０００を用いて行った。気孔数及び気孔率の結果を図４に示す。 The particle size of the SiC particles (average particle size, minimum particle size, maximum particle size) was calculated by observing the cross section of the refractory material by SEM and measuring all the SiC particles appearing within the range of 100 μm × 100 μm. As for the number of pores, the cross section of the refractory material was observed by SEM, and the pores within the range of 100 μm × 100 μm (pores of 0.05 μm or more and 25 μm or less) were visually counted. The porosity (apparent porosity) was measured in accordance with JIS R2205-1992. The cross-sectional SEM observation was performed using TM4000 manufactured by Hitachi High-Technologies Corporation. The results of the number of pores and the porosity are shown in FIG.
　成形性は、押出成形後の試料を目視で観察し、異常が確認されない試料を「◎」とし、変形が確認された試料を「〇」とし、変形及び切れ（シート切れ）が確認された試料に「△」、押出中にシート切れが頻繁に発生し、成形不能であった試料を「×」として評価した。 For formability, the sample after extrusion molding is visually observed, and the sample in which no abnormality is confirmed is marked with "◎", the sample in which deformation is confirmed is marked with "○", and the sample in which deformation and breakage (sheet breakage) are confirmed. The sample was evaluated as "Δ", and the sample that could not be molded due to frequent sheet breakage during extrusion was evaluated as "x".
　保形性は、押出成形後の試料を目視で観察し、設計公差の範囲内の試料を「◎」とし、設計公差からのずれが２ｍｍ未満の試料を「〇」とし、設計公差からのずれが２ｍｍ超の試料を「△」とし、実質的に測定不能（形状を維持していない）の試料を「×」として評価した。 For shape retention, visually observe the sample after extrusion molding, mark the sample within the range of the design tolerance as "◎", and mark the sample with a deviation from the design tolerance of less than 2 mm as "○", and deviate from the design tolerance. A sample with a value of more than 2 mm was evaluated as "Δ", and a sample that was substantially unmeasurable (the shape was not maintained) was evaluated as "x".
　図４に示すように、ＳｉＣ粒子の平均粒子径が１５μｍ以下であり、０．０５μｍ以上２５μｍ以下の気孔の数が１００個以上の試料（試料１～６）は、良好な強度（３００ＭＰａ以上）が得られることが確認された。また、ＳｉＣ粒子の最大粒子径が３０μｍ以下の試料（試料１～５）は、特に良好な強度（３５０ＭＰａ以上）が得られることが確認された。なお、ＳｉＣ粒子の最大粒子径が１５μｍ以下の試料（試料１～３）は、極めて良好な強度（４００ＭＰａ以上）が得られることが確認された。なお、良好な強度を示した試料（試料１～６）は、何れも最小粒子径が０．０５μｍ以上であり、見掛け気孔率が１％以下であった。なお、試料１～６は、試料７～９と比較して、何れも成形性、保形性が良好であることが確認された。 As shown in FIG. 4, samples (samples 1 to 6) having an average particle size of SiC particles of 15 μm or less and having 100 or more pores of 0.05 μm or more and 25 μm or less have good strength (300 MPa or more). Was confirmed to be obtained. Further, it was confirmed that particularly good strength (350 MPa or more) can be obtained for the samples (samples 1 to 5) having the maximum particle diameter of the SiC particles of 30 μm or less. It was confirmed that the samples (Samples 1 to 3) having a maximum particle size of SiC particles of 15 μm or less can obtain extremely good strength (400 MPa or more). The samples (Samples 1 to 6) showing good strength all had a minimum particle size of 0.05 μm or more and an apparent porosity of 1% or less. It was confirmed that Samples 1 to 6 had better moldability and shape retention than Samples 7 to 9.
　上述したように、試料１～３は、極めて高強度の耐火材が得れることが確認された。試料１～３と試料４～６について比較すると、試料１～３は、見掛け気孔率が０．５％以下であるという特徴を有している。この結果より、耐火材の見掛け気孔率を０．５％以下にすることにより、耐火材の強度をさらに向上させることができることが確認された。 As mentioned above, it was confirmed that samples 1 to 3 can obtain extremely high-strength refractory materials. Comparing Samples 1 to 3 and Samples 4 to 6, Samples 1 to 3 have a feature that the apparent porosity is 0.5% or less. From this result, it was confirmed that the strength of the refractory material can be further improved by setting the apparent porosity of the refractory material to 0.5% or less.
　上記実施例において、耐火材を利用したローラー、セッター、ビームの例を示したが、本明細書で開示する耐火材は、高温環境下で用いられる部品であれば、上記実施例以外の部品（製品）として利用することもできる。また、上記実施例では、円柱状のビームの例を示したが、ビームは角柱状であってもよい。 In the above embodiment, examples of a roller, a setter, and a beam using a refractory material have been shown, but the refractory material disclosed in the present specification is a part other than the above-mentioned embodiment as long as it is a part used in a high temperature environment. It can also be used as a product). Further, in the above embodiment, an example of a columnar beam is shown, but the beam may be a prismatic beam.
　以上、本発明の具体例を詳細に説明したが、これらは例示に過ぎず、請求の範囲を限定するものではない。請求の範囲に記載の技術には、以上に例示した具体例を様々に変形、変更したものが含まれる。また、本明細書または図面に説明した技術要素は、単独であるいは各種の組合せによって技術的有用性を発揮するものであり、出願時請求項記載の組合せに限定されるものではない。また、本明細書または図面に例示した技術は複数目的を同時に達成し得るものであり、そのうちの一つの目的を達成すること自体で技術的有用性を持つものである。 Although specific examples of the present invention have been described in detail above, these are merely examples and do not limit the scope of claims. The techniques described in the claims include various modifications and modifications of the specific examples exemplified above. Further, the technical elements described in the present specification or the drawings exhibit technical usefulness alone or in various combinations, and are not limited to the combinations described in the claims at the time of filing. In addition, the techniques exemplified in the present specification or the drawings can achieve a plurality of purposes at the same time, and achieving one of the purposes itself has technical usefulness.
１０：ローラー
１４：焼成用セッター
１６：加熱炉用ビーム 10: Roller 14: Firing setter 16: Beam for heating furnace

Claims (8)

  1. 　骨材としてＳｉＣ粒子を主体とし、前記ＳｉＣ粒子間に金属Ｓｉが含まれるＳｉ－ＳｉＣ質の耐火材であって、
    　前記ＳｉＣ粒子の平均粒子径が１５μｍ以下であり、
    　断面を観察したときに、０．０５μｍ以上２５μｍ以下の気孔が、１００μｍ×１００μｍの範囲に１００個以上存在している耐火材。     It is a SiC-SiC refractory material mainly composed of SiC particles as an aggregate and containing metallic Si between the SiC particles.
    The average particle size of the SiC particles is 15 μm or less.
    A refractory material in which 100 or more pores of 0.05 μm or more and 25 μm or less are present in a range of 100 μm × 100 μm when the cross section is observed.
  2. 　１００μｍ×１００μｍの範囲における、前記ＳｉＣ粒子の最大粒子径が３０μｍ以下である請求項１に記載の耐火材。 The refractory material according to claim 1, wherein the maximum particle size of the SiC particles is 30 μm or less in the range of 100 μm × 100 μm.
  3. 　１００μｍ×１００μｍの範囲における、前記ＳｉＣ粒子の最小粒子径が０．０５μｍ以上である請求項１または２に記載の耐火材。 The refractory material according to claim 1 or 2, wherein the minimum particle size of the SiC particles is 0.05 μm or more in the range of 100 μm × 100 μm.
  4. 　耐火材の見掛け気孔率が１％以下である請求項１から３のいずれか一項に記載の耐火材。 The refractory material according to any one of claims 1 to 3, wherein the refractory material has an apparent porosity of 1% or less.
  5. 　前記金属Ｓｉの割合が２０質量％以上６０質量％以下である請求項１から４のいずれか一項に記載の耐火材。 The refractory material according to any one of claims 1 to 4, wherein the proportion of the metallic Si is 20% by mass or more and 60% by mass or less.
  6. 　請求項１から５のいずれか一項に記載の耐火材によって形成されているローラー。 A roller formed of the refractory material according to any one of claims 1 to 5.
  7. 　請求項１から５のいずれか一項に記載の耐火材によって形成されている焼成用セッター。 A firing setter formed of the refractory material according to any one of claims 1 to 5.
  8. 　請求項１から５のいずれか一項に記載の耐火材によって形成されている加熱炉用ビーム。 A beam for a heating furnace formed of the refractory material according to any one of claims 1 to 5.
PCT/JP2021/014378 2020-09-07 2021-04-02 Refractory material WO2022049818A1 (en)

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