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JP3932405B2 - Method of joining silicon carbide heating elements - Google Patents
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JP3932405B2 - Method of joining silicon carbide heating elements - Google Patents

Method of joining silicon carbide heating elements Download PDF

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Publication number
JP3932405B2
JP3932405B2 JP14080297A JP14080297A JP3932405B2 JP 3932405 B2 JP3932405 B2 JP 3932405B2 JP 14080297 A JP14080297 A JP 14080297A JP 14080297 A JP14080297 A JP 14080297A JP 3932405 B2 JP3932405 B2 JP 3932405B2
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Prior art keywords
sic
silicon carbide
pressure
temperature
joining
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JP14080297A
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JPH10297976A (en
Inventor
浩明 花井
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Tokai Konetsu Kogyo Co Ltd
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Tokai Konetsu Kogyo Co Ltd
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Description

【0001】
【発明の属する技術分野】
本発明は、炭化珪素発熱体の発熱部と端部の接合方法に関するものである。
【0002】
【従来の技術】
従来、発熱体を製造するには、棒状のSiCの両端にSiを含浸させ端部とする方法が採られていた。しかしこの方法でつくられた発熱体の端部の比抵抗は発熱部の10%程度であり、該端部はそれだけ電力の損失となっていた。そこで省エネルギーの観点からこの電力損失を少なくするために、比抵抗の低い端部をつくり、これと発熱部を接合させるという技術が開発された。すなわち、該発熱体は、SiCからなる発熱部と、SiC−Siの複合材からなる端部とで構成されたものである。この技術により端部の電力損失を少なくすることができた。上述のようなSiCとSiC−Siの複合材を接合する方法としては、SiC,C,バインダーからなる接着剤を接合面に塗布して、窒素雰囲気中で高温(1900〜2100℃)に加熱し、溶融したSiと接着剤中のCと反応させる反応焼結接合が行われている。しかしこの方法は、処理温度が1900〜2100℃と高温なため、黒鉛炉等の特殊な装置が必要となってくる。またこの処理温度を低くする方法としては、炉内を減圧するという方法(特開昭63−17268号公報)がある。しかしこの方法だと圧力が低すぎる場合、端部のSiが蒸発してしまい、比抵抗が高くなってしまう。端部の比抵抗が上がれば発熱体として信頼性が損なわれてしまう。
【0003】
【発明が解決しようとする課題】
上述のように従来の接合法では、高温、高真空で処理できる炉のような特殊な設備がなければ、接合できないという問題があった。また低温で処理すると発熱体の端部の性能に問題があった。本発明の目的は黒鉛炉等の特殊な設備を必要とすることなく、かつ端部の性能を損ずることなしに、充分な強度を得ることができる接合方法を提供することにある。
【0004】
【課題を解決するための手段】
本発明の接合方法は、SiCからなる発熱部とSiC−Siの複合材からなる端部の接合面に、SiC,C,バインダーからなる接着剤を塗布し、これらを一定の減圧下(150〜1500Pa)に制御して、加熱(1450℃〜1600℃)し接合することを特徴とする。
【0005】
【発明の実施の形態】
本発明によれば、従来より500℃低い温度で処理することができる。もし圧力が1500Paを超えると、反応焼結が進まず接合部分の強度が不足してしまう。また15Pa未満では端部に含まれているSiが蒸発し比抵抗が上がってしまい、発熱体としての用をなさない。そこで15〜1500Paの圧力範囲で熱処理をすれば、強度不足の点も、端部の比抵抗が上がる点も解決できる。このように処理温度を下げることができることにより、黒鉛炉のような特殊な装置を使用する必要がなくなり、また接合に必要な電力量が少なくなり、大幅なコストダウンが可能となる。
【0006】
【実施例】
本発明を実施例により更に詳しく説明する。
(実施例1〜3、参考例1)SiCからなる発熱部(外径φ20、内径φ10、全長300mm)とSiC−Siの複合材からなる端部(外径φ20、内径φ10、全長300mm)を、SiCバインダーからなる接着剤で接合した。この接合体を圧力15〜1500Pa、温度1500℃で3時間処理し試験のサンプルとした。
(比較例1)実施例1〜4と同様の接合体を圧力3000Pa、温度1500℃で3時間処理し比較用のサンプルとした。表1に実施例1〜3、参考例1と比較例1の曲げ強度の結果を示す。
【0007】
【表1】

Figure 0003932405
この表の結果から、本発明の実施例1〜の圧力範囲内の条件で接合を実施して得られた接合体は、比較例1の接合体に対して良好な接合状態を有し、かつ充分な接合強度を有していた。
(実施例5〜7、参考例2)SiC−Siの複合材(遊離Si量12〜17%、外径φ20×内径φ10×全長100mm)を圧力15〜1500Pa、温度1500℃で3時間処理し、試験のサンプルとした。
(比較例2)実施例5〜7、参考例2と同じ複合材を圧力1.5Pa、温度1500℃で3時間処理し比較用のサンプルとした。表2に実施例5〜7、参考例2と比較例2のSi含有率と比抵抗を示す。
【0008】
【表2】
Figure 0003932405
この表の結果から、本発明の実施例5〜の圧力範囲内で熱処理されたSiC−Si複合材は、比較用の複合材比較例2に対して、Si含有量は多くなっている。これは圧力が15Pa未満になると、Siの蒸発が激しくなるためである。また比抵抗は実施例5〜の複合材に対して比較例2の複合材よりも低くなっている。これは実施例5〜の方が比較例2よりもSi含有量が多いためである。実施例5〜の複合材のような比抵抗であれば、発熱体の端部として利用することができる。また比較例2のように複合材の比抵抗が高いと、端部の電力損失が多くなり、発熱体に用いることができない。上記の実施例1〜および5〜、比較例1および2から炭化珪素発熱体の発熱部と端部を接合する場合、150〜1500Paの範囲で圧力調整を行えば、1450℃〜1600℃の温度で可能であるといえる。
【0009】
【発明の効果】
以上のとおり、本発明によれば炭化珪素発熱体の発熱部と端部を接合する際に、圧力を150〜1500Paの範囲で調整することにより、加熱処理温度は、従来より500℃低い1450〜1600℃の温度で行うことができる。このように低い温度で処理できるため、黒鉛炉といった特別な装置を必要としなくなった。また低い温度で処理できるため、電力消費量も少なくなり大幅なコストダウンが図れるようになる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for joining a heat generating portion and an end portion of a silicon carbide heating element.
[0002]
[Prior art]
Conventionally, in order to manufacture a heating element, a method has been adopted in which both ends of a rod-like SiC are impregnated with Si to form end portions. However, the specific resistance of the end portion of the heating element produced by this method is about 10% of that of the heating portion, and the end portion is a loss of electric power. Therefore, in order to reduce this power loss from the viewpoint of energy saving, a technology has been developed in which an end portion having a low specific resistance is formed and this is joined to a heat generating portion. That is, the heating element is composed of a heating part made of SiC and an end part made of a SiC-Si composite material. This technique can reduce the power loss at the end. As a method for joining the composite material of SiC and SiC-Si as described above, an adhesive composed of SiC, C, and a binder is applied to the joining surface and heated to a high temperature (1900 to 2100 ° C.) in a nitrogen atmosphere. In addition, reactive sintering bonding is performed in which molten Si reacts with C in the adhesive. However, this method requires a special apparatus such as a graphite furnace because the processing temperature is as high as 1900 to 2100 ° C. Further, as a method for lowering the treatment temperature, there is a method of reducing the pressure in the furnace (Japanese Patent Laid-Open No. 63-17268). However, with this method, when the pressure is too low, the Si at the end evaporates and the specific resistance becomes high. If the specific resistance at the end increases, the reliability of the heating element is impaired.
[0003]
[Problems to be solved by the invention]
As described above, the conventional bonding method has a problem that bonding cannot be performed without special equipment such as a furnace capable of processing at high temperature and high vacuum. Moreover, when it processed at low temperature, there existed a problem in the performance of the edge part of a heat generating body. An object of the present invention without requiring special equipment graphite furnace or the like, and the performance of the end without loss sly that is to provide a joining method capable of obtaining a sufficient strength.
[0004]
[Means for Solving the Problems]
In the bonding method of the present invention, an adhesive composed of SiC, C, and a binder is applied to a joint surface between an exothermic portion composed of SiC and an end portion composed of a SiC-Si composite material, and these are applied under a certain reduced pressure ( 150 to It is characterized by being heated (1450 ° C. to 1600 ° C.) and joined by being controlled at 1500 Pa).
[0005]
DETAILED DESCRIPTION OF THE INVENTION
According to the present invention, the treatment can be performed at a temperature lower by 500 ° C. than the conventional one. If the pressure exceeds 1500 Pa, the reaction sintering does not proceed and the strength of the joint portion is insufficient. On the other hand, if it is less than 15 Pa , Si contained in the end portion evaporates and the specific resistance increases, so that it cannot be used as a heating element. Therefore, if heat treatment is performed in a pressure range of 15 to 1500 Pa, both the insufficient strength and the specific resistance of the end portion can be solved. Since the processing temperature can be lowered in this manner, it is not necessary to use a special apparatus such as a graphite furnace, and the amount of electric power necessary for joining is reduced, which enables a significant cost reduction.
[0006]
【Example】
The present invention will be described in more detail with reference to examples.
(Examples 1 to 3, Reference Example 1 ) An exothermic part made of SiC (outer diameter φ20, inner diameter φ10, overall length 300 mm) and an end part made of a composite material of SiC-Si (outer diameter φ20, inner diameter φ10, overall length 300 mm) Bonding was performed using an adhesive composed of SiC , C , and binder. The joined body was treated at a pressure of 15 to 1500 Pa and a temperature of 1500 ° C. for 3 hours to obtain a test sample.
(Comparative Example 1) The same joined body as in Examples 1 to 4 was treated at a pressure of 3000 Pa and a temperature of 1500 ° C for 3 hours to obtain a sample for comparison. Table 1 shows the bending strength results of Examples 1 to 3, Reference Example 1 and Comparative Example 1 .
[0007]
[Table 1]
Figure 0003932405
From the results of this table, the joined body obtained by performing the joining under the conditions within the pressure range of Examples 1 to 3 of the present invention has a good joined state with respect to the joined body of Comparative Example 1, And it had sufficient joint strength.
(Examples 5 to 7, Reference Example 2 ) A SiC-Si composite material (free Si content 12 to 17%, outer diameter φ20 × inner diameter φ10 × total length 100 mm) was treated at a pressure of 15 to 1500 Pa and a temperature of 1500 ° C. for 3 hours. A test sample was obtained.
Comparative Example 2 The same composite material as in Examples 5 to 7 and Reference Example 2 was treated at a pressure of 1.5 Pa and a temperature of 1500 ° C. for 3 hours to obtain a sample for comparison. Table 2 shows the Si content and specific resistance of Examples 5 to 7, Reference Example 2 and Comparative Example 2 .
[0008]
[Table 2]
Figure 0003932405
From the results of this table, the SiC-Si composite material heat-treated within the pressure range of Examples 5 to 7 of the present invention has a higher Si content than the comparative composite material comparative example 2. This is because when the pressure is less than 15 Pa, the evaporation of Si becomes intense. The specific resistance is lower than the composite of Comparative Example 2 with respect to the composite materials of Examples 5-7. This is because Examples 5 to 7 have a higher Si content than Comparative Example 2. If the specific resistance, such as composite materials of Examples 5-7, can be utilized as an end of the heating element. Moreover, when the specific resistance of the composite material is high as in Comparative Example 2, the power loss at the end increases, and the composite cannot be used as a heating element. The above Examples 1 3 and 5-7, when bonding heat generating portion and the end portion of the silicon carbide heating elements from Comparative Examples 1 and 2, by performing pressure adjustment range of 150 ~1500Pa, 1450 ℃ ~1600 ℃ It can be said that it is possible at a temperature of
[0009]
【The invention's effect】
As described above, according to the present invention, when the heating portion and the end portion of the silicon carbide heating element are joined, the heat treatment temperature is 1450 to 1500 lower by 500 ° C. than before by adjusting the pressure in the range of 150 to 1500 Pa. It can be performed at a temperature of 1600 ° C. Since processing can be performed at such a low temperature, a special apparatus such as a graphite furnace is not required. Moreover, since the treatment can be performed at a low temperature, the power consumption is reduced and the cost can be significantly reduced.

Claims (1)

炭化珪素発熱体のSiCからなる発熱部と、SiC−Siの複合材からなる端部を、SiC,C,バインダーからなる接合剤で接合し、比抵抗の低い端部を得る方法において、接合を、圧力が150〜1500Paの減圧下1450〜1600℃の温度で加熱処理することにより行うことを特徴とする炭化珪素発熱体の接合方法。In a method of joining a heat generating part made of SiC of a silicon carbide heating element and an end part made of a SiC-Si composite material with a bonding agent made of SiC, C, and a binder to obtain an end part having a low specific resistance. under a reduced pressure of pressure 0.99 ~1500Pa, method of joining silicon carbide heating elements, characterized in that by heating at a temperature of from 1,450 to 1,600 ° C..
JP14080297A 1997-04-24 1997-04-24 Method of joining silicon carbide heating elements Expired - Fee Related JP3932405B2 (en)

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JP3932405B2 true JP3932405B2 (en) 2007-06-20

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JP5187579B2 (en) * 2008-12-01 2013-04-24 東海高熱工業株式会社 Method for manufacturing end portion of silicon carbide heating element

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