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JP2603586B2 - Gas inlet pipe for sintering furnace and method of manufacturing the same - Google Patents

Gas inlet pipe for sintering furnace and method of manufacturing the same

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Publication number
JP2603586B2
JP2603586B2 JP31969392A JP31969392A JP2603586B2 JP 2603586 B2 JP2603586 B2 JP 2603586B2 JP 31969392 A JP31969392 A JP 31969392A JP 31969392 A JP31969392 A JP 31969392A JP 2603586 B2 JP2603586 B2 JP 2603586B2
Authority
JP
Japan
Prior art keywords
gas
sintering furnace
protective layer
furnace
gas inlet
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.)
Expired - Lifetime
Application number
JP31969392A
Other languages
Japanese (ja)
Other versions
JPH06158108A (en
Inventor
寛 渋谷
等 蓮野
Original Assignee
東京タングステン株式会社
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Priority to JP31969392A priority Critical patent/JP2603586B2/en
Publication of JPH06158108A publication Critical patent/JPH06158108A/en
Application granted granted Critical
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Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明は、焼結炉に用いられるガ
ス導入管に関し、特に、水素ガスなどの還元性ガスを焼
結炉内に導入することに適したガス導入管に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a gas introduction pipe used in a sintering furnace, and more particularly to a gas introduction pipe suitable for introducing a reducing gas such as hydrogen gas into a sintering furnace.

【0002】[0002]

【従来の技術】従来のガス導入管を備えた焼結炉を図2
に示す。図2において、この焼結炉は、炉体30内に備
えられ、被処理物90を収容する炉体壁40と、炉体壁
40に挿入されたガス導入管50および熱電温度計60
と、炉体壁40内に備えられたヒータ70とを有してい
る。炉体壁40は、保温材としてのカーボンフェルトか
ら成る。ガス導入管50は、カーボンから成り、その一
端に炉体壁40内で導入ガス80を導入する開口部を有
し、他端が導入ガス80を導入するための配管とネジ等
の継手により係合する形状を呈している。また、熱電温
度計60は、炉体壁40内に測温部を有している。
2. Description of the Related Art FIG. 2 shows a conventional sintering furnace equipped with a gas inlet tube.
Shown in In FIG. 2, the sintering furnace is provided in a furnace body 30, and includes a furnace body wall 40 that accommodates an object to be processed 90, a gas introduction pipe 50 inserted into the furnace body wall 40, and a thermoelectric thermometer 60.
And a heater 70 provided in the furnace body wall 40. The furnace wall 40 is made of carbon felt as a heat insulating material. The gas introduction pipe 50 is made of carbon, has an opening at one end for introducing the introduction gas 80 in the furnace body wall 40, and the other end is connected to a pipe for introducing the introduction gas 80 by a joint such as a screw. It has a matching shape. Further, the thermoelectric thermometer 60 has a temperature measuring unit inside the furnace body wall 40.

【0003】ところで、被処理物90は、一般に、炭化
物や炭化物を含む合金など少なくとも一部に炭素を含む
材質であり、高温下の焼結工程においては、被処理物9
0から炭素が輝散する。このため、炉体壁40、ガス導
入管50およびヒータ70などの焼結炉の各部材には、
輝散した炭素と結合するような金属から成るものは使用
できない。このことと耐熱性および加工性とを考慮し
て、従来の焼結炉の部材には、カーボン材を使用するこ
とが普通である。
[0003] The workpiece 90 is generally a material containing carbon at least in part, such as a carbide or an alloy containing a carbide.
From 0, carbon scatters. For this reason, each member of the sintering furnace such as the furnace body wall 40, the gas introduction pipe 50, and the heater 70 includes:
Metals that bind to scattered carbon cannot be used. In consideration of this, heat resistance and workability, it is common to use a carbon material for the members of the conventional sintering furnace.

【0004】[0004]

【発明が解決しようとする課題】前述の導入ガス80と
して、例えば、水素ガスを使用した場合、500℃〜9
00℃にまで及ぶ焼結工程中に、カーボン材から成る焼
結炉の各部材に対して水素ガスが化学式1に示す化学反
応を起こす。焼結工程においては、炉体壁40内を減圧
(例えば、10-1〜10-2Torr)することがあり、この
減圧下では反応生成物の蒸気圧が上昇し、化学反応はよ
り顕著となる。さらに、この導入ガス80等に不純物と
して水分が存在する場合には、化学式2に示すような化
学反応も併せて起こる。
When, for example, hydrogen gas is used as the above-mentioned introduced gas 80, the temperature is 500.degree.
During the sintering process up to 00 ° C., the hydrogen gas causes a chemical reaction shown in Chemical Formula 1 to each member of the sintering furnace made of the carbon material. In the sintering step, the pressure inside the furnace body wall 40 may be reduced (for example, 10 -1 to 10 -2 Torr). Become. Further, when moisture is present as an impurity in the introduced gas 80 or the like, a chemical reaction as shown in Chemical Formula 2 also occurs.

【0005】[0005]

【化1】 C+2H→CH(gas)Embedded image C + 2H 2 → CH 4 (gas)

【0006】[0006]

【化2】 C+HO→CO(gas)Embedded image C + H 2 O → CO (gas)

【0007】焼結炉の各部材のうち、特にガス導入管5
0では、水素ガス(導入ガス80)の流れに直接接触す
る構造であるから、これらの化学反応が顕著に起こり、
開口部が短くなったり、管壁に穴が開いたりなどの損耗
が生ずる。例えば、従来のガス導入管(外径が12mm、
内径が6mm、長さが370mm)を備えた焼結炉を900
時間稼働させた実験では、導入ガスの放出口が長さ約1
50mm損耗した結果が得られている。
[0007] Among the members of the sintering furnace, in particular, the gas introduction pipe 5
In the case of 0, since the structure is in direct contact with the flow of hydrogen gas (introduced gas 80), these chemical reactions occur remarkably,
Wear such as shortening of the opening or opening of the tube wall occurs. For example, a conventional gas inlet pipe (outer diameter 12 mm,
900 sintering furnace with 6mm inner diameter and 370mm length)
In the experiment that was operated for hours, the outlet of the introduced gas was
A result of 50 mm wear was obtained.

【0008】このガス導入管50の損耗により、水素ガ
スが本来の位置からずれて放出されると、炉体壁40に
水素ガスが直接接触して炉体壁40にも損耗が生じ、こ
の結果、炉体壁40の保温機能が低下するという問題点
がある。
When the hydrogen gas is released from its original position due to the wear of the gas introduction pipe 50, the hydrogen gas comes into direct contact with the furnace body wall 40 and the furnace body wall 40 is also worn. However, there is a problem that the heat retaining function of the furnace body wall 40 is reduced.

【0009】また、ガス導入管50の損耗により、水素
ガスが熱電温度計60の測温部に向かって放出される場
合には、正確な温度計測が行えなくなるという問題点が
ある。
Further, when hydrogen gas is discharged toward the temperature measuring part of the thermoelectric thermometer 60 due to the wear of the gas introduction pipe 50, there is a problem that accurate temperature measurement cannot be performed.

【0010】さらに、損耗したガス導入管50や炉体壁
40の交換、修理を行うために、焼結炉の稼働を停止さ
せなければならず、保守上の扱いが面倒なばかりか、経
済面でも不利であるという問題点がある。
Further, in order to replace or repair the worn gas introduction pipe 50 and the furnace body wall 40, the operation of the sintering furnace must be stopped. However, there is a problem that it is disadvantageous.

【0011】本発明の課題は、水素ガスや混入水分との
化学反応を起こしにくい焼結炉用ガス導入管を提供する
ことである。
An object of the present invention is to provide a gas inlet pipe for a sintering furnace, which hardly causes a chemical reaction with hydrogen gas or mixed moisture.

【0012】[0012]

【課題を解決するための手段】本発明によれば、カーボ
ン材による筒状の基体から成り、焼結炉内に還元性の導
入ガスを導入する焼結炉用ガス導入管において、前記基
体の表面のうち少なくとも前記導入ガスに曝される部分
に、Al2 3 およびZrO2 のうちの一方から成る保
護層を形成したことを特徴とする焼結炉用ガス導入管が
得られる。
According to the present invention, there is provided a sintering furnace gas inlet pipe for introducing a reducing introducing gas into a sintering furnace, comprising a tubular base made of a carbon material. A gas introduction pipe for a sintering furnace, wherein a protective layer made of one of Al 2 O 3 and ZrO 2 is formed on at least a portion of the surface exposed to the introduction gas, is obtained.

【0013】本発明によればまた、前記焼結炉用ガス導
入管の製造方法において、容射法、化学気相蒸着法、お
よび水ガラスを用いた塗布法のうちのいずれかの方法に
より、前記基体の表面のうち少なくとも前記導入ガスに
曝される部分に、前記保護層を形成することを特徴とす
る焼結炉用ガス導入管の製造方法が得られる。
According to the present invention, in the method for producing a gas inlet tube for a sintering furnace, any one of a spraying method, a chemical vapor deposition method, and a coating method using water glass may be used. A method for manufacturing a gas inlet tube for a sintering furnace, wherein the protective layer is formed on at least a portion of the surface of the substrate exposed to the introduced gas.

【0014】[0014]

【実施例】以下、本発明による焼結炉用ガス導入管の実
施例を説明する。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of a gas inlet pipe for a sintering furnace according to the present invention will be described below.

【0015】[実施例1]図1は、本発明による焼結炉
用ガス導入管を示す概略断面図である。図1において、
本焼結炉用ガス導入管は、一端11と他端12とを有す
る筒形を呈し、カーボン材から成る基体10と、基体1
0の表面に形成されたAl2 3 から成る保護層20と
から構成されている。基体10は、一端11と他端12
との間に延び、内壁14により規定される中央孔と、ガ
ス配管との接続のために他端12側の外壁13に形成さ
れたネジ山を有している。保護層20は、一端11、外
壁13のうちネジ山を除く部分、内壁14全面に形成さ
れている。
Embodiment 1 FIG. 1 is a schematic sectional view showing a gas inlet pipe for a sintering furnace according to the present invention. In FIG.
The gas introduction pipe for a sintering furnace has a cylindrical shape having one end 11 and the other end 12, and has a base 10 made of a carbon material and a base 1
0 and a protective layer 20 made of Al 2 O 3 formed on the surface of the substrate. The base 10 has one end 11 and the other end 12
And has a central hole defined by an inner wall 14 and a thread formed in an outer wall 13 on the other end 12 side for connection with a gas pipe. The protective layer 20 is formed on one end 11, a portion of the outer wall 13 excluding the thread, and the entire inner wall 14.

【0016】次に、この焼結炉用ガス導入管の製造方法
を説明する。
Next, a method of manufacturing the gas inlet tube for a sintering furnace will be described.

【0017】まず、カーボン材から成る筒体(例えば、
外径が12mm、内径が6mm、長さが370mm)を用意
し、続いて、真空中の溶射法により、この筒体の一端、
外壁および内壁に、Al2 3 から成る保護層20を形
成する。この後、外壁の他端側にネジ山(例えば、M1
2で長さ10mm)を形成する。以上のようにして、図1
に示す焼結炉用ガス導入管が製造できた。
First, a cylindrical body made of carbon material (for example,
An outer diameter of 12 mm, an inner diameter of 6 mm, and a length of 370 mm) were prepared.
A protective layer 20 made of Al 2 O 3 is formed on the outer and inner walls. Then, a screw thread (for example, M1
2 to form a length of 10 mm). As described above, FIG.
The gas introduction pipe for a sintering furnace shown in FIG.

【0018】得られた焼結炉用ガス導入管を、図2に示
す焼結炉に組み込み、焼結炉を稼働させた。組み込みの
際には、その一端11側を炉体壁40内に挿入し、他端
12側のネジ山を導入ガス80を導入するための配管に
設けた継手と係合させた。焼結炉を稼働させたところ、
1800時間経過しても、本焼結炉用ガス導入管は、そ
の長さおよび肉厚共に損耗が確認されなかった。
The obtained gas inlet tube for a sintering furnace was incorporated into the sintering furnace shown in FIG. 2, and the sintering furnace was operated. At the time of assembling, one end 11 side was inserted into the furnace body wall 40, and the thread on the other end 12 side was engaged with a joint provided in a pipe for introducing the introduction gas 80. When the sintering furnace was operated,
Even after 1800 hours, the length and thickness of the gas introduction pipe for the sintering furnace were not found to be worn.

【0019】尚、実施例1においては、保護層を真空中
の溶射法により形成しているが、真空中に限らず大気圧
中における溶射法でもよい。ただし、真空中における溶
射法の方が、形成される保護層が緻密な表面となり、例
えば、10-1〜10-2Torr下における水素ガスに対して
も反応を起こしにくい。
In the first embodiment, the protective layer is formed by a thermal spraying method in a vacuum. However, the protective layer is not limited to a vacuum but may be a thermal spraying method in an atmospheric pressure. However, in the thermal spraying method in a vacuum, the formed protective layer has a dense surface, and does not easily react with hydrogen gas at, for example, 10 -1 to 10 -2 Torr.

【0020】[実施例2]図1に示す焼結炉用ガス導入
管の保護層20を、化学気相蒸着(CVD)法により形
成した。製造方法を以下に説明する。
Example 2 The protective layer 20 of the gas inlet pipe for a sintering furnace shown in FIG. 1 was formed by a chemical vapor deposition (CVD) method. The manufacturing method will be described below.

【0021】前述したカーボン材から成る筒体(外径が
12mm、内径が6mm、長さが370mm)を用意し、この
筒体を約1000℃に保持した状態で、Alチップに塩
素ガスを接触させて約250℃で生成したAl2 3
CO2 ガスとを同時に放射し、筒体の一端、外壁および
内壁に、Al2 3 を形成する。この後、外壁の他端側
にネジ山(M12で長さ10mm)を形成する。以上のよ
うにして、実施例2による焼結炉用ガス導入管が製造で
きた。
A tubular body (outside diameter: 12 mm, inside diameter: 6 mm, length: 370 mm) made of the carbon material described above was prepared, and chlorine gas was brought into contact with the Al chip while keeping the tubular body at about 1000 ° C. Then, Al 2 O 3 and CO 2 gas generated at about 250 ° C. are simultaneously radiated to form Al 2 O 3 on one end, outer wall and inner wall of the cylinder. Thereafter, a thread (M12, 10 mm long) is formed on the other end of the outer wall. As described above, the sintering furnace gas inlet tube according to Example 2 was manufactured.

【0022】このCVD法によれば、本実施例のように
導入管の径が比較的小さい場合(外径が12mm、内径が
6mm)であっても、溶射法に比べて保護層が形成しやす
い。
According to this CVD method, even when the diameter of the introduction tube is relatively small (outer diameter is 12 mm and inner diameter is 6 mm) as in this embodiment, a protective layer is formed as compared with the thermal spraying method. Cheap.

【0023】[実施例3]前述したカーボン材から成る
筒体(外径が12mm、内径が6mm、長さが370mm)の
一端、外壁および内壁に、Al2 3 と水ガラスとの混
合物を塗布し、加熱乾燥させて、Al2 3 から成る保
護層20を形成することも可能である。尚、Al2 3
と水ガラスとの混合物を塗布した状態の筒体を図2に示
す焼結炉に組み付け、焼結炉の空焼き(導入ガス80を
導入しない状態でヒータ70により加熱)を行えば、よ
り簡単に保護層20を形成できる。
Example 3 A mixture of Al 2 O 3 and water glass was applied to one end, an outer wall and an inner wall of a tubular body (outside diameter: 12 mm, inside diameter: 6 mm, length: 370 mm) made of the carbon material described above. It is also possible to form the protective layer 20 made of Al 2 O 3 by applying and drying by heating. In addition, Al 2 O 3
It is easier to assemble the cylindrical body coated with the mixture of water and water glass into the sintering furnace shown in FIG. 2 and to bake the sintering furnace (heating by the heater 70 without introducing the introduction gas 80). The protective layer 20 can be formed on the substrate.

【0024】尚、実施例1〜3においては、カーボン材
から成る基体に、Al2 3 から成る保護層を形成した
が、本発明における保護層はこれに限定されず、ZrO
2 から成るものでもよい。
In Examples 1 to 3, the protective layer made of Al 2 O 3 was formed on the substrate made of carbon material. However, the protective layer in the present invention is not limited to this.
It may be composed of two .

【0025】[0025]

【発明の効果】本発明による焼結炉用ガス導入管は、カ
ーボン材による筒状の基体の表面のうち少なくとも還元
性の導入ガスに曝される部分に、Al2 3 およびZr
2 のうちの一方から成る保護層が形成されているた
め、焼結工程中に水素ガスや水分と化学反応を起こすこ
とがない。特に、炉内を10-2〜10-4Torrに減圧し、
ここに水素ガスを10-1〜10-2Torrになるまで導入し
て、焼結雰囲気を形成するような焼結工程であっても、
ガス導入管の開口部が短くなるなどの損耗がなく、水素
ガスは本来の位置から導入されるため、水素ガスが炉体
壁に向けて放出されて炉体壁が損耗して炉体機能が低下
することがない。また、熱電温度計の測温部に向けて放
出されることもなく、焼結炉の温度計測を正確に行え
る。
The gas introduction pipe for a sintering furnace according to the present invention has a structure in which at least a portion of the surface of a cylindrical substrate made of carbon material which is exposed to a reducing introduction gas has Al 2 O 3 and Zr.
Since the protective layer made of one of O 2 is formed, no chemical reaction occurs with hydrogen gas or moisture during the sintering process. In particular, the pressure in the furnace is reduced to 10 -2 to 10 -4 Torr,
Here, even in a sintering step in which a hydrogen gas is introduced until the pressure becomes 10 -1 to 10 -2 Torr to form a sintering atmosphere,
There is no wear such as shortening of the opening of the gas introduction pipe, and hydrogen gas is introduced from the original position.Hydrogen gas is released toward the furnace body wall, and the furnace body wall is worn and the furnace body function is reduced. It does not drop. Further, the temperature of the sintering furnace can be accurately measured without being emitted toward the temperature measuring section of the thermoelectric thermometer.

【0026】さらに、ガス導入管や炉体壁の交換、修理
を頻繁に行う必要がなく、焼結炉の保守を簡単かつ経済
的に行える。
Further, the sintering furnace can be easily and economically maintained without the need for frequent replacement and repair of the gas inlet pipe and the furnace body wall.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明の実施例による焼結炉用ガス導入管を示
す縦断面図である。
FIG. 1 is a longitudinal sectional view showing a gas inlet pipe for a sintering furnace according to an embodiment of the present invention.

【図2】本実施例および従来例によるガス導入管が用い
られる焼結炉を示す概略図である。
FIG. 2 is a schematic view showing a sintering furnace using gas introduction pipes according to the present embodiment and a conventional example.

【符号の説明】[Explanation of symbols]

10 基体 11 一端 12 他端 13 外壁 14 内壁 20 保護層 30 炉体 40 炉体壁 50 ガス導入管 60 熱電温度計 70 ヒータ 80 導入ガス 90 被処理物 DESCRIPTION OF SYMBOLS 10 Base 11 One end 12 Other end 13 Outer wall 14 Inner wall 20 Protective layer 30 Furnace body 40 Furnace body wall 50 Gas introduction pipe 60 Thermoelectric thermometer 70 Heater 80 Introduced gas 90 Workpiece

Claims (2)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 カーボン材による筒状の基体から成り、
焼結炉内に還元性の導入ガスを導入する焼結炉用ガス導
入管において、前記基体の表面のうち少なくとも前記導
入ガスに曝される部分に、Al2 3 およびZrO2
うちの一方から成る保護層を形成したことを特徴とする
焼結炉用ガス導入管。
1. A tubular base made of a carbon material,
In a sintering furnace gas introduction pipe for introducing a reducing introduction gas into a sintering furnace, at least a portion of the surface of the substrate exposed to the introduction gas includes one of Al 2 O 3 and ZrO 2. A gas introduction pipe for a sintering furnace, comprising a protective layer made of:
【請求項2】 請求項1に記載の焼結炉用ガス導入管の
製造方法において、容射法、化学気相蒸着法および水
ガラスを用いた塗布法のうちのいずれかの方法により、
前記基体の表面のうち少なくとも前記導入ガスに曝され
る部分に、前記保護層を形成することを特徴とする焼結
炉用ガス導入管の製造方法。
2. A gas introduction pipe for a sintering furnace according to claim 1.
In the manufacturing method, spraying method, chemical vapor deposition method , and by any one of the coating method using water glass,
A method for manufacturing a gas inlet tube for a sintering furnace, comprising forming the protective layer on at least a portion of the surface of the substrate exposed to the introduced gas.
JP31969392A 1992-11-30 1992-11-30 Gas inlet pipe for sintering furnace and method of manufacturing the same Expired - Lifetime JP2603586B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP31969392A JP2603586B2 (en) 1992-11-30 1992-11-30 Gas inlet pipe for sintering furnace and method of manufacturing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP31969392A JP2603586B2 (en) 1992-11-30 1992-11-30 Gas inlet pipe for sintering furnace and method of manufacturing the same

Publications (2)

Publication Number Publication Date
JPH06158108A JPH06158108A (en) 1994-06-07
JP2603586B2 true JP2603586B2 (en) 1997-04-23

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CN117570725B (en) * 2024-01-16 2024-03-29 湘潭新大粉末冶金技术有限公司 A sintering furnace inlet and exhaust reversing ventilation system

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JPH06158108A (en) 1994-06-07

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