JPH11236267A - Oxidation resistant silicon carbide-silicon composite material and its production - Google Patents
Oxidation resistant silicon carbide-silicon composite material and its productionInfo
- Publication number
- JPH11236267A JPH11236267A JP10096525A JP9652598A JPH11236267A JP H11236267 A JPH11236267 A JP H11236267A JP 10096525 A JP10096525 A JP 10096525A JP 9652598 A JP9652598 A JP 9652598A JP H11236267 A JPH11236267 A JP H11236267A
- Authority
- JP
- Japan
- Prior art keywords
- sic
- composite material
- oxidation resistant
- oxidation
- production
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、近年、炉用構造材
が部材として用いられてきたＳｉＣ−Ｓｉ複合材におい
て、酸素濃度が低いアクティブ酸化領域で用いられる耐
酸化性ＳｉＣ−Ｓｉ複合材に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an oxidation-resistant SiC-Si composite material used in an active oxidation region having a low oxygen concentration in a SiC-Si composite material for which a structural material for a furnace has been used as a member in recent years. .
【０００２】[0002]
【従来の技術】近年、１０００℃〜１３００℃の温度領
域の加熱炉の構成部材としてＳｉＣ−Ｓｉ複合材の使用
が飛躍的に伸びている。ＳｉＣ−Ｓｉ複合材は、高温強
度や耐酸化性に非常に優れた材料で、耐久性の面からロ
ーラ、梁、支柱、さや、棚板、吊り棒などの用途に広く
採用されている。これらの用途には、再結晶質ＳｉＣ、
反応焼結ＳｉＣ、ＳｉＣ常圧焼結体が以前から用いられ
てきた。再結晶質ＳｉＣは耐酸化性、高温強度で反応焼
結ＳｉＣは、寸法精度や形状、ＳｉＣ常圧焼結体はコス
ト面などで欠点を有しており、ユーザーの要求仕様を十
分に満たすまでに至らなかった。ＳｉＣ−Ｓｉ複合材
は、ＳｉＣ体の気孔の中にＳｉを溶融含浸して得られる
ため、ほとんど気孔がなく、耐熱性、高温強度、耐熱衝
撃性、耐摩耗性、耐酸化性を具備しており、更に比較的
安価で製造できる材料であるため、今後大きく伸びる材
料として脚光を浴びている。2. Description of the Related Art In recent years, the use of a SiC-Si composite material as a component of a heating furnace in a temperature range of 1000.degree. The SiC-Si composite material is a material having excellent high-temperature strength and oxidation resistance, and is widely used in applications such as rollers, beams, columns, pods, shelves, and hanging bars from the viewpoint of durability. These applications include recrystallized SiC,
Reaction sintered SiC and normal pressure sintered SiC have been used for some time. Recrystallized SiC is resistant to oxidation and has high temperature strength. Reaction sintered SiC has drawbacks in terms of dimensional accuracy and shape, and SiC atmospheric pressure sintered bodies have disadvantages in terms of cost. Did not reach. Since the SiC-Si composite material is obtained by melting and impregnating Si into the pores of the SiC body, it has almost no pores and has heat resistance, high temperature strength, thermal shock resistance, abrasion resistance, and oxidation resistance. In addition, since it is a material that can be manufactured relatively inexpensively, it has been spotlighted as a material that will greatly expand in the future.
【０００３】[0003]
【発明が解決しようとする課題】ＳｉＣ−Ｓｉ複合材
は、緻密でＳｉが含有されているため酸化雰囲気の使用
において、表面にＳｉＯ２が生成し保護膜となり、素材
中にＯ２の拡散がみられず、非常に耐酸化性が優れてい
る。しかし、酸素濃度が低い領域（数％レベル以下のＯ
２濃度）の場合 ２Ｓｉ＋Ｏ２→２ＳｉＯ↑ の反応がおこり、ガス体のＳｉＯが発生する。このＳｉ
Ｏは保護膜にならないだけでなく、発生したＳｉＯガス
は炉内で被加熱物などと反応し、悪影響を与える問題が
発生していた。（アクティブ酸化） つまり、ＳｉＣ−Ｓｉ複合材の表面に露出しているフリ
ーのＳｉは非常に活性な状態となっており、微量なＯ２
と反応し、ＳｉＯガスを発生させるものである。例え
ば、各種の焼成容器において、容器内が密閉状態となる
と容易に酸素濃度が低い状態となり、ＳｉＯガスが発生
し、容器内に充填した被加熱物と反応し、得率を著しく
低下させ、大きな問題となっていた。本発明の目的は、
酸素濃度の低い領域でも十分な耐酸化性を持ったＳｉＣ
−Ｓｉ複合材及びその製造方法を提供することにある。The SiC-Si composite material is dense and contains Si, so that when an oxidizing atmosphere is used, SiO 2 is generated on the surface to serve as a protective film, and the diffusion of O 2 into the material is suppressed. It is not observed and has very excellent oxidation resistance. However, in the region where the oxygen concentration is low (O 2
2 concentration), a reaction of 2Si + O 2 → 2SiO ↑ occurs to generate gaseous SiO. This Si
O not only does not act as a protective film, but the generated SiO gas reacts with an object to be heated in a furnace, causing a problem of adverse effects. (Active oxide) that is, Si free exposed on the surface of the SiC-Si composite has a very active state, a minute amount of O 2
Reacts with and generates SiO gas. For example, in various firing containers, when the inside of the container becomes a closed state, the oxygen concentration easily becomes a low state, SiO gas is generated, reacts with the heated object filled in the container, the yield is significantly reduced, and Had been a problem. The purpose of the present invention is
SiC with sufficient oxidation resistance even in regions with low oxygen concentration
-Si composite material and its manufacturing method.
【０００４】[0004]
【課題を解決するための手段】すなわち本発明は、Ｓｉ
Ｃ７０〜９０重量％とＳｉ３０〜１０重量％とからなる
ＳｉＣ−Ｓｉ複合材の表面に露出して存在するＳｉをＳ
ｉ３Ｎ４に転化させたことを特徴とする。更に、骨材と
してのＳｉＣ体にＳｉを溶融含浸して得られたＳｉＣ−
Ｓｉ複合材を窒素雰囲気中で１４００〜２１００℃の温
度で熱処理することを特徴とする。Means for Solving the Problems That is, the present invention relates to a Si
The Si which is exposed on the surface of the SiC-Si composite material composed of 70 to 90% by weight of C and 30 to 10% by weight of Si
It is characterized by being converted to i 3 N 4 . Furthermore, SiC-body obtained by melting and impregnating Si into an SiC body as an aggregate is obtained.
The Si composite material is heat-treated at a temperature of 1400 to 2100 ° C. in a nitrogen atmosphere.
【０００５】[0005]
【発明の実施の形態】本発明の母材となるＳｉＣ−Ｓｉ
複合材は、ＳｉＣが７０〜９０重量％とＳｉが３０〜１
０重量％の組成割合からなる複合セラミックスが用いら
れる。ＳｉＣが７０重量％未満、Ｓｉが３０重量％を越
える場合は、含浸したＳｉが多いため耐クリープ特性や
耐摩耗性が低下する。また、ＳｉＣが９０重量％を越
え、Ｓｉが１０重量％を下回ると残存する気孔が多くな
って、強度低下や耐酸化性の低下を招くこととなる。本
発明において、表面の露出したＳｉのみＳｉ３Ｎ４に転
化させれば良く、表面層部分の数μｍ程度で十分であ
る。内部のＳｉは、ＳｉＯガスの発生には関与しない。
又、転化させる方法は、様々考えられるが窒素雰囲気中
で１４００℃以上の温度で熱処理することで容易に転化
できる。反応時間も短時間で十分である。２１００℃を
越えると短時間でもＳｉの抜ける量が多くなり、気孔が
大きくなるため好ましくない。DESCRIPTION OF THE PREFERRED EMBODIMENTS SiC-Si serving as a base material of the present invention
The composite material contains 70 to 90% by weight of SiC and 30 to 1% of Si.
A composite ceramic having a composition ratio of 0% by weight is used. If the content of SiC is less than 70% by weight and the content of Si exceeds 30% by weight, the amount of impregnated Si is large, so that the creep resistance and wear resistance are reduced. On the other hand, if the content of SiC exceeds 90% by weight and the content of Si is less than 10% by weight, the number of remaining pores increases, leading to a decrease in strength and a decrease in oxidation resistance. In the present invention, it is sufficient that only the exposed surface Si is converted into Si 3 N 4 , and the surface layer portion of about several μm is sufficient. Internal Si does not contribute to the generation of SiO gas.
Although various conversion methods are conceivable, conversion can be easily performed by heat treatment at a temperature of 1400 ° C. or more in a nitrogen atmosphere. A short reaction time is sufficient. If the temperature exceeds 2100 ° C., the amount of Si coming out increases even in a short time, and pores increase, which is not preferable.
【０００６】[0006]
【実施例】ＳｉＣ粉末からなる成形体を窒素雰囲気中
で、２０００℃の温度で加熱し、Ｓｉを溶融含浸した。
組成割合として、ＳｉＣ８０重量％とＳｉ２０重量％と
の複合材料を得た。この複合材料を１８００℃の温度で
１時間窒素雰囲気中で熱処理し、本発明に係る複合材を
得た。該複合材を１〜２％のＯ２濃度のＮ２雰囲気中、
１３００℃の温度の炉内に曝した。結果を表１に示す。
なお、比較のため、熱処理の無いもの、１３００℃での
熱処理、２１５０℃での熱処理したものについても評価
した。EXAMPLE A molded body made of SiC powder was heated at a temperature of 2000 ° C. in a nitrogen atmosphere to melt and impregnate Si.
As a composition ratio, a composite material of 80% by weight of SiC and 20% by weight of Si was obtained. This composite material was heat-treated at a temperature of 1800 ° C. for 1 hour in a nitrogen atmosphere to obtain a composite material according to the present invention. The composite material is placed in an N 2 atmosphere having an O 2 concentration of 1 to 2%,
It was exposed in a furnace at a temperature of 1300 ° C. Table 1 shows the results.
For comparison, those without heat treatment, those with heat treatment at 1300 ° C., and those with heat treatment at 2150 ° C. were also evaluated.
【０００７】[0007]
【表１】 表１の実施例に示すように本発明は、ＳｉＯによる酸化
もなく、又、Ｓｉの減少もないことから、気孔率の増大
もないため、耐酸化性や強度劣化もみられない材料とい
える。[Table 1] As shown in the examples of Table 1, the present invention can be said to be a material having neither oxidation resistance nor deterioration in strength because there is no oxidation due to SiO and there is no decrease in Si, so there is no increase in porosity.
【０００８】[0008]
【発明の効果】以上のとおり、本発明のＳｉＣ−Ｓｉ複
合材は酸素濃度の低い領域でもＳｉＯガスの発生を抑制
し、十分な耐酸化性を得ることができる。窒素雰囲気中
で熱処理することで表面のＳｉをＳｉ３Ｎ４に転化させ
ることは非常に容易で、更にコスト的にも大きな負担と
ならないため、１０００〜１３００℃の温度領域の加熱
炉の構成部材、例えばローラ、梁、支柱、さや、棚板、
吊り棒などに広く利用できるものである。As described above, the SiC-Si composite material of the present invention can suppress generation of SiO gas even in a region having a low oxygen concentration, and can obtain sufficient oxidation resistance. It is very easy to convert Si on the surface to Si 3 N 4 by heat treatment in a nitrogen atmosphere, and it does not impose a large burden on cost. Therefore, components of a heating furnace in a temperature range of 1000 to 1300 ° C. , For example, rollers, beams, struts, pods, shelves,
It can be widely used for hanging bars and the like.
Claims (2)
０重量％とからなるＳｉＣ−Ｓｉ複合材の表面に露出し
て存在するＳｉをＳｉ３Ｎ４に転化させたことを特徴と
する耐酸化性ＳｉＣ−Ｓｉ複合材。1. 70% to 90% by weight of SiC and 30% to 1% of Si
0 wt% and the oxidation resistance SiC-Si composites the Si existing exposed on the surface of the SiC-Si composite, characterized in that was converted into Si 3 N 4 consisting of.
させたＳｉＣ−Ｓｉ複合材を窒素雰囲気中で１４００℃
〜２１００℃の温度で熱処理する耐酸化性ＳｉＣ−Ｓｉ
複合材の製造方法。2. An SiC-Si composite material obtained by melting and impregnating Si into an SiC body as an aggregate is heated to 1400 ° C. in a nitrogen atmosphere.
Oxidation resistant SiC-Si heat treated at a temperature of ~ 2100 ° C
Manufacturing method of composite material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10096525A JPH11236267A (en) | 1998-02-24 | 1998-02-24 | Oxidation resistant silicon carbide-silicon composite material and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10096525A JPH11236267A (en) | 1998-02-24 | 1998-02-24 | Oxidation resistant silicon carbide-silicon composite material and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11236267A true JPH11236267A (en) | 1999-08-31 |
Family
ID=14167566
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10096525A Pending JPH11236267A (en) | 1998-02-24 | 1998-02-24 | Oxidation resistant silicon carbide-silicon composite material and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11236267A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060004513A (en) * | 2004-07-09 | 2006-01-12 | 엘지전자 주식회사 | Composite material fabricating method for high voltage igniter |
| JP2006151719A (en) * | 2004-11-26 | 2006-06-15 | Bridgestone Corp | Method of manufacturing silicon carbide sintered compact for heater |
| KR20100086527A (en) * | 2009-01-23 | 2010-08-02 | 한국과학기술연구원 | Ceramic body coated with diamond layer and preparation method thereof using two-phase composite |
-
1998
- 1998-02-24 JP JP10096525A patent/JPH11236267A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060004513A (en) * | 2004-07-09 | 2006-01-12 | 엘지전자 주식회사 | Composite material fabricating method for high voltage igniter |
| JP2006151719A (en) * | 2004-11-26 | 2006-06-15 | Bridgestone Corp | Method of manufacturing silicon carbide sintered compact for heater |
| KR20100086527A (en) * | 2009-01-23 | 2010-08-02 | 한국과학기술연구원 | Ceramic body coated with diamond layer and preparation method thereof using two-phase composite |
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