JPH09159366A - Heating furnace and heat treatment method of metal powder - Google Patents
Heating furnace and heat treatment method of metal powderInfo
- Publication number
- JPH09159366A JPH09159366A JP34550195A JP34550195A JPH09159366A JP H09159366 A JPH09159366 A JP H09159366A JP 34550195 A JP34550195 A JP 34550195A JP 34550195 A JP34550195 A JP 34550195A JP H09159366 A JPH09159366 A JP H09159366A
- Authority
- JP
- Japan
- Prior art keywords
- metal powder
- muffle
- heat treatment
- carbon
- atmosphere
- 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
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、一酸化ケイ素ガス
の発生する雰囲気で使用しても強度劣化のない加熱炉及
びこれを用いた金属ケイ素粉末等の金属粉末の熱処理方
法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a heating furnace which does not deteriorate in strength even when used in an atmosphere in which silicon monoxide gas is generated, and a heat treatment method for metal powder such as metal silicon powder using the heating furnace.
【０００２】[0002]
【従来の技術及び発明が解決しようとする課題】従来、
金属ケイ素粉末を、その窒化反応の促進のため予め不活
性ガス雰囲気下又は減圧下で熱処理し、下記反応 ＳｉＯ2（ｓ）＋Ｓｉ（ｓ）→２ＳｉＯ（ｇ） により脱酸素を行い、このように脱酸素した金属ケイ素
粉末を窒化ケイ素原料とすることが知られている。2. Description of the Related Art
In order to accelerate the nitriding reaction, the metallic silicon powder is heat-treated in advance under an inert gas atmosphere or under reduced pressure, and deoxidized by the following reaction SiO 2 (s) + Si (s) → 2SiO (g). It is known to use deoxidized metal silicon powder as a silicon nitride raw material.
【０００３】しかしながら、上記金属ケイ素粉末の脱酸
素に用いる加熱炉は、一般に炉内壁が黒鉛にて形成され
ており、このため上記反応で発生する一酸化ケイ素と黒
鉛とで下記反応 ＳｉＯ（ｇ）＋２Ｃ（ｓ）→ＳｉＣ（ｓ）＋ＣＯ（ｇ） が生じ、炉内壁を形成する黒鉛材料の寿命が低下する要
因になっていた。However, in the heating furnace used for deoxidizing the metal silicon powder, the inner wall of the furnace is generally made of graphite. Therefore, the following reaction SiO (g) occurs between the silicon monoxide generated in the above reaction and graphite. + 2C (s) → SiC (s) + CO (g) was generated, which was a factor of shortening the life of the graphite material forming the inner wall of the furnace.
【０００４】このため、このような問題に対しては、黒
鉛材料のかさ密度等の物性を変えることによって延命を
行っているが、黒鉛材料が劣化することは避けられず、
この点の解決が望まれている。For this reason, the problem is solved by prolonging the life by changing the physical properties such as the bulk density of the graphite material, but the deterioration of the graphite material is unavoidable.
A solution to this point is desired.
【０００５】この場合、黒鉛材料の表面をＳｉＣやガラ
ス質炭素等で化学的に被覆することは有効な手段である
が、その表面被覆層の一部が剥がれると、そこから酸化
が進展したり、コスト高となるなどの問題がある。In this case, it is an effective means to chemically coat the surface of the graphite material with SiC, glassy carbon, or the like, but if a part of the surface coating layer is peeled off, oxidation may proceed from there. There are problems such as high cost.
【０００６】本発明は上記事情に鑑みなされたもので、
一酸化ケイ素ガスの存在する雰囲気下で金属粉末を熱処
理しても強度劣化のない加熱炉及び該加熱炉を用いた金
属粉末の熱処理方法を提供することを目的とする。The present invention has been made in view of the above circumstances,
An object of the present invention is to provide a heating furnace that does not deteriorate in strength even if the metal powder is heat-treated in an atmosphere containing silicon monoxide gas, and a method for heat-treating the metal powder using the heating furnace.
【０００７】[0007]
【課題を解決するための手段及び発明の実施の形態】本
発明者らは、上記目的を達成するため鋭意検討を行った
結果、炭素を母体とする炭素繊維強化炭素材質よりなる
マッフルを用い、この中で金属ケイ素粉末等の金属粉末
を熱処理した場合、一酸化ケイ素ガスが発生しても、マ
ッフルに割れや劣化を生じることなく強度を保持できる
ことを知見した。Means for Solving the Problems and Modes for Carrying Out the Invention As a result of intensive studies to achieve the above object, the present inventors have used a muffle made of a carbon fiber-reinforced carbon material having carbon as a matrix, It has been found that when a metal powder such as a metal silicon powder is heat-treated therein, the strength can be maintained without cracking or deterioration of the muffle even if silicon monoxide gas is generated.
【０００８】即ち、発生する一酸化ケイ素ガスは、マッ
フルの内側で炭素と反応して炭素が炭化ケイ素に変質
し、その結果、従来の炭素材料では、外側で引張り応
力、内側で圧縮応力がかかり、残留歪みにより割れ及び
劣化が生じるが、上記炭素繊維強化炭素材料は気孔が多
いため、一酸化ケイ素と反応して全体が炭化ケイ素に変
質するものの、高温高強度及び高靭性を維持でき、強度
劣化がないことを知見し、本発明をなすに至ったもので
ある。That is, the generated silicon monoxide gas reacts with carbon inside the muffle to transform the carbon into silicon carbide. As a result, in the conventional carbon material, tensile stress is applied to the outside and compressive stress is applied to the inside. However, cracks and deterioration occur due to residual strain, but since the carbon fiber reinforced carbon material has many pores, it reacts with silicon monoxide and transforms into silicon carbide as a whole, but it is possible to maintain high temperature high strength and high toughness. The present inventors have completed the present invention by finding that there is no deterioration.
【０００９】従って、本発明は、炉内部に炭素を母体と
する炭素繊維強化炭素基材のマッフルを備えてなること
を特徴とする加熱炉、及び金属粉末を一酸化ケイ素ガス
が存在する雰囲気下で熱処理するに際し、上記金属粉末
を炭素繊維強化炭素基材のマッフル内に入れて熱処理す
ることを特徴とする金属粉末の熱処理方法を提供する。Therefore, according to the present invention, a heating furnace characterized in that a muffle of a carbon fiber reinforced carbon base material having carbon as a base material is provided inside the furnace, and a metal powder in an atmosphere in which silicon monoxide gas is present. A heat treatment method for a metal powder, characterized in that the heat treatment is carried out by placing the metal powder in a muffle of a carbon fiber reinforced carbon substrate.
【００１０】以下、本発明につき更に詳しく説明する
と、本発明の加熱炉は、炉内部に炭素繊維強化炭素基材
のマッフルを備えたものである。この場合、この炭素繊
維強化炭素材料としては市販のものを使用することがで
きる。The present invention will be described in more detail below. The heating furnace of the present invention is provided with a muffle of a carbon fiber reinforced carbon base material inside the furnace. In this case, a commercially available carbon fiber reinforced carbon material can be used.
【００１１】その形状は筒状、角状など、適宜選定され
るが、マッフルは炉内部の加熱部にこの加熱部内壁を覆
うように内側に配置し、炉内壁を一酸化ケイ素ガスから
保護するようにすることが好ましい。The shape of the muffle is appropriately selected such as a cylindrical shape or a square shape, but the muffle is arranged inside the furnace so as to cover the inner wall of the heating section and protects the inner wall of the furnace from the silicon monoxide gas. It is preferable to do so.
【００１２】本発明においては、このようなマッフルの
内側に金属粉末を入れて熱処理するが、特に好適には、
金属ケイ素粉末をヘリウム、アルゴン等の不活性ガス雰
囲気下又は減圧（通常０．０１〜１０Ｔｏｒｒ）下に熱
処理し、この金属ケイ素粉末中の酸素を除去する目的に
有効である。この熱処理温度は、種々選定されるが、上
記金属ケイ素粉末の脱酸素の目的のためには１１００〜
１４１０℃の範囲で熱処理を行うことが好ましい。In the present invention, metal powder is put into the inside of such a muffle and heat-treated, but particularly preferably,
It is effective for the purpose of removing oxygen in the metal silicon powder by heat-treating the metal silicon powder in an atmosphere of an inert gas such as helium or argon or under reduced pressure (usually 0.01 to 10 Torr). The heat treatment temperature is selected variously, but for the purpose of deoxidizing the metal silicon powder, 1100 to
It is preferable to perform heat treatment in the range of 1410 ° C.
【００１３】このような熱処理、特に金属ケイ素粉末の
不活性ガス雰囲気下又は減圧下での加熱により、上述し
た通り、 Ｓｉ＋ＳｉＯ2→２ＳｉＯ（ｇ） の反応で一酸化ケイ素ガスが発生し、このガスは炭素を
母体とする炭素繊維強化炭素製マッフルと反応してこれ
を炭化ケイ素化するが、上述したようにマッフルの強度
は維持でき、強度劣化が少ないため、割れ等の不都合な
く長時間安定して使用することができ、多数回の繰り返
し使用に耐えるものである。By such heat treatment, particularly heating of the metallic silicon powder in an inert gas atmosphere or under reduced pressure, silicon monoxide gas is generated by the reaction of Si + SiO 2 → 2SiO (g) as described above. Reacts with a carbon fiber reinforced carbon muffle having carbon as a base material to convert it into silicon carbide.However, as described above, the strength of the muffle can be maintained and the strength deterioration is small, so that it will be stable for a long time without causing problems such as cracking. It can be used for many times and can be used repeatedly.
【００１４】[0014]
【実施例】以下、実施例と比較例を示し、本発明を具体
的に説明するが、本発明は下記の実施例に制限されるも
のではない。EXAMPLES The present invention will be described below in detail with reference to examples and comparative examples, but the present invention is not limited to the following examples.
【００１５】〔実施例〕平均粒子径が４μｍ以上１０μ
ｍ以下の金属ケイ素粉末２５ｋｇを窒化ケイ素製トレイ
に仕込み、炭素を母体とする直径６３０ｍｍの炭素繊維
強化炭素製マッフル内に静置した。なお、マッフルは、
図１，２の加熱炉の加熱部内側に配置した。なお、図中
１は加熱炉本体、２はヒーター、３はマッフル、４は試
料台、５はトレイである。[Example] Average particle size of 4 μm or more and 10 μm
25 kg of metal silicon powder having a particle size of m or less was charged into a silicon nitride tray and allowed to stand still in a carbon fiber-reinforced carbon muffle having a carbon matrix and a diameter of 630 mm. The muffle is
It was arranged inside the heating part of the heating furnace shown in FIGS. In the figure, 1 is a heating furnace main body, 2 is a heater, 3 is a muffle, 4 is a sample stand, and 5 is a tray.
【００１６】上記仕込み後、炉内を１０Ｔｏｒｒ以下の
減圧下、１３５０℃にて２時間加熱を行った。After the above charging, the inside of the furnace was heated at 1350 ° C. for 2 hours under a reduced pressure of 10 Torr or less.
【００１７】以上の操作を繰り返し行った結果、１４バ
ッチ目の重量増は６５％で炭化ケイ素の存在が確認され
たが、１００バッチを過ぎてもマッフルに割れは生じな
かった。As a result of repeating the above operation, the weight increase of the 14th batch was 65%, and the presence of silicon carbide was confirmed, but cracks did not occur in the muffle even after 100 batches.
【００１８】〔比較例１〕直径６３０ｍｍ、厚さ１０ｍ
ｍのＣＩＰ成形品炭素製マッフルを用いた以外は実施例
と同様に操作した結果、マッフルは６バッチ目で割れが
生じた。[Comparative Example 1] Diameter 630 mm, thickness 10 m
As a result of operating in the same manner as in the example except that a carbon muffle of CIP molded product of m was used, cracks were generated in the muffle in the sixth batch.
【００１９】〔比較例２〕直径６３０ｍｍ、厚さ１０ｍ
ｍの押出成形品炭素製マッフルを用いた以外は実施例と
同様に操作した結果、マッフルは１０バッチ目に割れが
生じた。[Comparative Example 2] Diameter 630 mm, thickness 10 m
As a result of operating in the same manner as in Example except that the carbon muffle extruded product of m was used, the muffle was cracked at the 10th batch.
【００２０】[0020]
【発明の効果】本発明によれば、例えば金属ケイ素粉末
などの不活性ガス雰囲気下又は減圧下での熱処理により
発生する一酸化ケイ素ガスに対する耐久性が高く、マッ
フル寿命が大幅に伸びるため、このような金属ケイ素粉
末等の金属粉末の熱処理を有効に行うことができる。According to the present invention, the durability against silicon monoxide gas generated by heat treatment in an atmosphere of an inert gas such as metallic silicon powder or under reduced pressure is high, and the muffle life is greatly extended. The heat treatment of the metal powder such as the metal silicon powder can be effectively performed.
【図１】実施例で用いた加熱炉の断面図である。FIG. 1 is a cross-sectional view of a heating furnace used in an example.
【図２】図１のＡ−Ａ線に沿った断面図である。FIG. 2 is a sectional view taken along line AA of FIG.
１ 加熱炉本体 ２ ヒーター ３ マッフル 1 Heating furnace body 2 Heater 3 Muffle
───────────────────────────────────────────────────── フロントページの続き (72)発明者 進藤 敏彦 群馬県安中市磯部２丁目13番１号 信越化 学工業株式会社精密機能材料研究所内 ──────────────────────────────────────────────────の Continuing on the front page (72) Inventor Toshihiko Shindo 2-13-1 Isobe, Annaka-shi, Gunma Prefecture Shin-Etsu Chemical Industry Co., Ltd.
Claims (4)
炭素基材のマッフルを備えてなることを特徴とする加熱
炉。1. A heating furnace comprising a muffle of a carbon fiber reinforced carbon base material having carbon as a base material inside the furnace.
の金属粉末熱処理用である請求項１記載の加熱炉。2. The heating furnace according to claim 1, which is for heat treatment of metal powder in an atmosphere in which silicon monoxide gas is present.
雰囲気下で熱処理するに際し、上記金属粉末を炭素繊維
強化炭素基材のマッフル内に入れて熱処理することを特
徴とする金属粉末の熱処理方法。3. A heat treatment method for a metal powder, which comprises heat-treating the metal powder in a muffle of a carbon fiber-reinforced carbon base material when heat-treating the metal powder in an atmosphere containing silicon monoxide gas. .
理温度が１１００〜１４１０℃である請求項３記載の方
法。4. The method according to claim 3, wherein the metal powder is metal silicon powder and the heat treatment temperature is 1100 to 1410 ° C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34550195A JPH09159366A (en) | 1995-12-08 | 1995-12-08 | Heating furnace and heat treatment method of metal powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34550195A JPH09159366A (en) | 1995-12-08 | 1995-12-08 | Heating furnace and heat treatment method of metal powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09159366A true JPH09159366A (en) | 1997-06-20 |
Family
ID=18377016
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34550195A Pending JPH09159366A (en) | 1995-12-08 | 1995-12-08 | Heating furnace and heat treatment method of metal powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH09159366A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009091195A (en) * | 2007-10-09 | 2009-04-30 | Shin Etsu Chem Co Ltd | Apparatus and method for producing silicon monoxide |
| JP2013121915A (en) * | 2013-01-25 | 2013-06-20 | Shin-Etsu Chemical Co Ltd | Apparatus and method for producing silicon monoxide |
| WO2013141024A1 (en) * | 2012-03-22 | 2013-09-26 | Shin-Etsu Chemical Co., Ltd. | Method and system for the production of silicon oxide deposit |
-
1995
- 1995-12-08 JP JP34550195A patent/JPH09159366A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009091195A (en) * | 2007-10-09 | 2009-04-30 | Shin Etsu Chem Co Ltd | Apparatus and method for producing silicon monoxide |
| WO2013141024A1 (en) * | 2012-03-22 | 2013-09-26 | Shin-Etsu Chemical Co., Ltd. | Method and system for the production of silicon oxide deposit |
| US9790095B2 (en) | 2012-03-22 | 2017-10-17 | Shin-Etsu Chemical Co., Ltd. | Method and system for the production of silicon oxide deposit |
| JP2013121915A (en) * | 2013-01-25 | 2013-06-20 | Shin-Etsu Chemical Co Ltd | Apparatus and method for producing silicon monoxide |
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