JPH11304998A - Ceramic thermoelectric conversion element, its production method and its contacting method - Google Patents
Ceramic thermoelectric conversion element, its production method and its contacting methodInfo
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- JPH11304998A JPH11304998A JP11663898A JP11663898A JPH11304998A JP H11304998 A JPH11304998 A JP H11304998A JP 11663898 A JP11663898 A JP 11663898A JP 11663898 A JP11663898 A JP 11663898A JP H11304998 A JPH11304998 A JP H11304998A
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- Prior art keywords
- thermoelectric conversion
- conversion element
- type
- sic
- temperature
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E20/00—Combustion technologies with mitigation potential
- Y02E20/16—Combined cycle power plant [CCPP], or combined cycle gas turbine [CCGT]
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、２００℃以上の廃
熱を高効率で電気に変換して再利用できることから、一
般産業廃熱や原子力発電所、高温ガス炉等の高温部から
の熱を有効に電力に変換利用する際に使用されるセラミ
ック製の熱電変換素子、その製造方法及びその接合方法
に関する。BACKGROUND OF THE INVENTION The present invention is capable of converting waste heat of 200.degree. C. or more to electricity with high efficiency and reusing the same. Therefore, the present invention relates to general industrial waste heat and heat from high temperature parts such as nuclear power plants and high temperature gas furnaces. TECHNICAL FIELD The present invention relates to a thermoelectric conversion element made of ceramic used for effectively converting and converting electric power into electric power, a manufacturing method thereof, and a joining method thereof.
【０００２】[0002]
【従来の技術】従来の４００℃以上の高温熱の熱電気変
換素子用合金を原子炉熱変換に用いる場合下記の問題が
ある。即ち、原子炉を高温熱源とした場合、原子炉から
の放射線により、従来材である熱電変換素子合金では、
放射線損傷による材料特性の劣化や素子用合金のメン
テナンスの際の放射化による作業員の被曝の問題が考
えられる。また、高温雰囲気での熱電変換素子自身の
高温酸化による材料劣化と、さらには従来材での根本的
問題として高温での発電効率が低い点が上げられる。2. Description of the Related Art When a conventional alloy for a thermoelectric conversion element having a high temperature of 400.degree. That is, when the nuclear reactor is a high-temperature heat source, the radiation from the nuclear reactor causes the conventional thermoelectric conversion element alloy to:
The problem of deterioration of material properties due to radiation damage and exposure of workers due to activation during maintenance of element alloys may be considered. In addition, material degradation due to high-temperature oxidation of the thermoelectric conversion element itself in a high-temperature atmosphere and a fundamental problem with conventional materials include low power generation efficiency at high temperatures.
【０００３】[0003]
【発明が解決しようとする課題】本発明では、ＳｉＣ
（Ｐ型）／ＳｉＣ（Ｎ型）、及びＳｉＣ（Ｎ型）／Ｂ4
Ｃ（Ｐ型）セラミックス製のＰ／Ｎ型熱電変換素子を開
発することにより、上記の従来法に関わる問題点につい
て下記の対策を講じてある。SUMMARY OF THE INVENTION In the present invention, SiC
(P-type) / SiC (N-type) and SiC (N-type) / B 4
By developing a P / N type thermoelectric conversion element made of C (P type) ceramics, the following countermeasures have been taken for the above-mentioned problems associated with the conventional method.
【０００４】即ち、上記の放射線損傷については、Ｓ
ｉＣ等の放射線損傷に強い特性を有する材料を基本材料
に用いることによって熱電変換素子の長寿命化を図って
いる。That is, regarding the above radiation damage, S
By using a material having a property resistant to radiation damage such as iC as a basic material, the life of the thermoelectric conversion element is extended.
【０００５】さらに、上記の放射化による作業員の被
曝についても、放射化の極めて少ないＳｉＣ等のセラミ
ックス製の熱電変換素子を用いている。また、高温雰囲
気での熱電変換素子自身の上記の高温酸化性について
は、高温での耐酸化性の優れたＳｉＣ等のセラミックス
製の熱電変換素子を用いている。[0005] Further, with respect to the exposure of workers due to the above-mentioned activation, a thermoelectric conversion element made of ceramic such as SiC, which has very little activation, is used. Regarding the high-temperature oxidation property of the thermoelectric conversion element itself in a high-temperature atmosphere, a thermoelectric conversion element made of ceramics such as SiC having excellent oxidation resistance at high temperatures is used.
【０００６】上記の発電効率については、本発明のＳ
ｉＣ等のセラミック製の熱電変換素子材料では、高温に
なるに従って材料の電気抵抗が合金とは逆に減少（改
善）していく特性を有するとともに、放射線照射によっ
ても同じく電気抵抗が減少していることになる。従っ
て、原子炉を熱源とした場合、原子炉から発生する高温
熱とともに放射線照射により電気変換効率が向上するこ
とになる。[0006] Regarding the power generation efficiency described above, S
The thermoelectric conversion element material made of ceramic such as iC has a characteristic that the electric resistance of the material decreases (improves) in reverse to the alloy as the temperature increases, and the electric resistance also decreases by irradiation with radiation. Will be. Therefore, when the nuclear reactor is used as the heat source, the electric conversion efficiency is improved by the radiation irradiation together with the high-temperature heat generated from the nuclear reactor.
【０００７】[0007]
【課題を解決するための手段】従来、ＳｉＣ等のセラミ
ック製材料は、耐熱構造材料や機能材料（絶縁材料）と
してしか利用されなかったのに対して、本発明は、Ｓｉ
Ｃ等のセラミック製材料が熱電変換素子（又は半導体）
に代わり得るとの特性を利用して電気材料としての新し
い利用分野を提案している。本発明は原子力分野のみな
らず一般利用に展開することになればＳｉＣ等のセラミ
ック製材料の普及、及び環境汚染防止等における効果が
期待できる。Conventionally, ceramic materials such as SiC have been used only as heat-resistant structural materials or functional materials (insulating materials).
Ceramic materials such as C are thermoelectric conversion elements (or semiconductors)
It proposes a new field of application as an electrical material by utilizing the characteristic that it can be used instead of. The present invention can be expected to be effective not only in the field of nuclear power but also in general use, in terms of the spread of ceramic materials such as SiC and the effect of preventing environmental pollution.
【０００８】即ち、本発明は、原子炉等の高温で放射線
が強い場所で、高効率で熱−電気変換できる熱電変換素
子であり、その電気抵抗が１０オームｃｍ以下の抵抗で
かつ起電力が数ｍＶ以上の耐熱性セラミックス材で製作
される熱電変換素子であり、それが多孔質で熱伝導率が
低く成績係数Ｚの高いものである。That is, the present invention relates to a thermoelectric conversion element capable of performing thermo-electric conversion with high efficiency in a place such as a nuclear reactor where the temperature is high and radiation is strong, the electric resistance of which is less than 10 ohm cm and the electromotive force is lower. A thermoelectric conversion element made of a heat-resistant ceramic material of several mV or more, which is porous, has a low thermal conductivity and a high coefficient of performance Z.
【０００９】本発明のＰ型熱電変換素子は、ＳｉＣ＋ボ
ロンカーバイト（１〜１００ｗｔ％）をアルゴン又は窒
素ガス雰囲気中で焼結することにより製造され、又本発
明のＮ型熱電変換素子は、ＳｉＣ＋Ｃ（１〜１０ｗｔ
％）又はＳｉ（１〜１０ｗｔ％）をアルゴン雰囲気又は
窒素ガス雰囲気中で焼結することにより製造される。そ
の熱電変換素子とリード線間はＴｉ系ロウ材を使用して
とを接合される。The P-type thermoelectric conversion element of the present invention is manufactured by sintering SiC + boron carbide (1 to 100 wt%) in an argon or nitrogen gas atmosphere. SiC + C (1-10wt
%) Or Si (1 to 10 wt%) in an argon atmosphere or a nitrogen gas atmosphere. The thermoelectric conversion element and the lead wire are joined together using a Ti-based brazing material.
【００１０】[0010]
【発明の実施の形態】なお、表１には、上記ＳｉＣ系の
出発原料を使用した場合の焼結体の密度、焼結条件、Ｐ
／Ｎ型判定結果及ぶ室温における電気抵抗が示されてい
る。出発原料を２２７３Ｋ以下で焼結するとＮ型、２４
７３Ｋ以上ではＰ型の熱電変換素子（半導体）的性質を
示す。しかしながら、室温における電気抵抗値は高い。DESCRIPTION OF THE PREFERRED EMBODIMENTS Table 1 shows the density, sintering conditions and P of the sintered body when the above-mentioned SiC-based starting material was used.
The / N type determination result and the electrical resistance at room temperature are shown. When the starting material is sintered at 2273K or lower, it becomes N-type, 24
Above 73K, it exhibits the properties of a P-type thermoelectric conversion element (semiconductor). However, the electrical resistance at room temperature is high.
【００１１】[0011]
【表１】 [Table 1]
【００１２】図１には、各種混合粉末の焼結温度、電気
抵抗及びＰ／Ｎ型特性が示されており、図１からみる
と、焼結温度が上がるに従ってＮ型からＰ型に、且つβ
からαに変態するが、それにボロンカーバイト（Ｂ
4Ｃ）を添加することによりＰ型の電気抵抗が下がり、
また、ＣやＳｉを添加した場合には２４７５Ｋの高温焼
結で低抵抗のＮ型半導体が製作できることが分かる。こ
れらの結果から、Ｐ／Ｎ型熱電変換素子を効率的に製作
するための方法として下記の手順が考えられる。FIG. 1 shows the sintering temperature, electric resistance and P / N type characteristics of various mixed powders. From FIG. 1, it can be seen that as the sintering temperature increases, the type changes from N type to P type, and β
To α, but boron carbide (B
4 ) By adding C), the electrical resistance of the P-type decreases,
Also, it can be seen that when C or Si is added, an N-type semiconductor having a low resistance can be manufactured by sintering at a high temperature of 2475K. From these results, the following procedure is considered as a method for efficiently manufacturing a P / N type thermoelectric conversion element.
【００１３】超微粒β−ＳｉＣ粉末＋ボロンカーバイ
ト（１〜１０ｗｔ％）粉末を成形プレス容器に入れ、次
にその上に超微粒β−ＳｉＣ粉末＋Ｓｉ（１〜１０ｗｔ
％）の混合粉末を入れ、プレスして成型体を製作する。The ultrafine β-SiC powder + boron carbide (1-10 wt%) powder is put into a molding press container, and then the ultrafine β-SiC powder + Si (1-10 wt%) is placed thereon.
%) And pressed to produce a molded body.
【００１４】その成型体を２４７３Ｋで焼結すること
によってＰ型とＮ型が直接接合したＰ／Ｎ熱電素子を作
ることができる。By sintering the molded body at 2473 K, a P / N thermoelectric element in which a P-type and an N-type are directly joined can be manufactured.
【００１５】図２には、Ｐ型熱電変換素子における混合
粉末中のボロンカーバイトの添加量、焼結温度及び焼結
体の電気抵抗が示されており、図２から、その混合粉末
中のボロン量を増やすと焼結体の電気抵抗が低下り、ま
た焼結温度を高温化すると電気抵抗が下がることが示さ
れている。FIG. 2 shows the addition amount of boron carbide in the mixed powder, the sintering temperature and the electric resistance of the sintered body in the P-type thermoelectric conversion element. It is shown that when the amount of boron is increased, the electric resistance of the sintered body decreases, and when the sintering temperature is increased, the electric resistance decreases.
【００１６】図３には、Ｎ型熱電変換素子の高温におけ
る電気抵抗の変化と温度との関係が示されており、図３
から、高温になるに従ってその電気抵抗が下がる傾向が
みられる。FIG. 3 shows the relationship between the change in the electric resistance of the N-type thermoelectric conversion element at a high temperature and the temperature.
Therefore, the electric resistance tends to decrease as the temperature increases.
【００１７】図４には、製作したＳｉＣ（Ｎ型）／Ｂ４
Ｃ（Ｐ型）のＰ／Ｎ型熱電変換素子の高温における起電
力特性が示されており、図４から、製作したＳｉＣ（Ｎ
型）／Ｂ4Ｃ（Ｐ型）のＰ／Ｎ型熱電変換素子では、温
度が上がるに従って起電圧が上昇する傾向が認められ
る。また、６００Ｋで約１００ｍＶの高い起電圧を観測
した。以下、本発明を実施例に基づいて具体的に説明す
る。FIG. 4 shows the fabricated SiC (N-type) / B4
The electromotive force characteristics of the C (P-type) P / N-type thermoelectric conversion element at a high temperature are shown, and FIG.
(Type) / B 4 C (p-type) P / N-type thermoelectric conversion element has a tendency to increase the electromotive voltage as the temperature increases. In addition, a high electromotive voltage of about 100 mV was observed at 600K. Hereinafter, the present invention will be specifically described based on examples.
【００１８】[0018]
【実施例】超微細ＳｉＣ（β型）粉末（粒径＜１ミクロ
ンｍ）を用いて下記焼結プロセス処理を実施することに
より、表１に示すようなＳｉＣのＰ型及びＮ型熱電変換
素子（半導体）が得られることを明らかにした。EXAMPLE A P-type and N-type thermoelectric conversion element of SiC as shown in Table 1 was obtained by performing the following sintering process using ultra-fine SiC (β type) powder (particle size <1 μm). (Semiconductor) was obtained.
【００１９】（焼結プロセス処理） プリフォーム；超微粒β−ＳｉＣ粉末を成形プレスで
直径φ１５×厚み１０ｍｍｔ以上のプリフォーム材を大
気中で２０００ｋｇｆで１５分間以上加圧成形した。(Sintering Process Treatment) Preform: An ultrafine β-SiC powder was formed by pressing a preform material having a diameter of φ15 and a thickness of 10 mmt or more at 2,000 kgf for 15 minutes or more in the atmosphere by a molding press.
【００２０】成形；上記の処理材をゴム等の不浸透
材で覆って、静水圧２００ＭＰａに１５分以上加えて成
形した。Molding: The above treated material was covered with an impervious material such as rubber and molded by applying a hydrostatic pressure of 200 MPa for 15 minutes or more.
【００２１】焼結；この成形体をアルゴン雰囲気（圧
力大気圧〜５ｋｇ／ｃｍ2）で（１）Ｎ型熱電変換素子
（半導体）を作る際は、２０００℃〜２１００℃で、
（２）Ｐ型熱電変換素子（半導体）を作る場合は２２０
０℃以上で焼結した。この際の昇温速度は、５〜１０℃
／分、最高温度保持時間２０分〜５時間、降温速度１〜
２℃／分であった。Sintering: (1) When forming the N-type thermoelectric conversion element (semiconductor) in an argon atmosphere (atmospheric pressure to 5 kg / cm 2 ) at 2000 to 2100 ° C.
(2) 220 for making a P-type thermoelectric conversion element (semiconductor)
Sintered above 0 ° C. The heating rate at this time is 5 to 10 ° C.
/ Min, maximum temperature holding time 20 minutes to 5 hours, temperature drop rate 1
2 ° C./min.
【００２２】表１では、各Ｐ及びＮ型の室温における電
気抵抗計測値も示してある。これによると、製作した材
料はそれぞれ１０ｋオーム以上の高い電気抵抗を示して
いる。そこで、室温における電気抵抗を下げるために下
記添加材を添加することにより作成した。Table 1 also shows the measured electrical resistance of each P and N type at room temperature. According to this, each of the manufactured materials has a high electric resistance of 10 kΩ or more. Therefore, in order to reduce the electric resistance at room temperature, the following additive was added to make the electrode.
【００２３】Ｐ型熱電変換素子を得る場合： 超微粒β
−ＳｉＣ粉末＋ボロンカーバイト（１〜１００ｗｔ％）
をアルゴン若しくは窒素雰囲気中で焼結処理する。その
焼結条件は上記〜に従う。When a P-type thermoelectric conversion element is obtained: ultra-fine particles β
-SiC powder + boron carbide (1 to 100 wt%)
Is sintered in an argon or nitrogen atmosphere. The sintering conditions are as described above.
【００２４】Ｎ型熱電変換素子を得る場合： 超微粒子
β−ＳｉＣ粉末を窒素雰囲気中で焼結する。超微粒β−
ＳｉＣ粉末＋Ｃ（１〜１０ｗｔ％）をアルゴン若しくは
窒素雰囲気中で焼結する。又は超微粒β−ＳｉＣ粉末＋
Ｓｉ（１〜１０ｗｔ％）をアルゴン若しくは窒素雰囲気
中で焼結する。その焼結条件は上記〜に従う。When obtaining an N-type thermoelectric conversion element: Ultrafine β-SiC powder is sintered in a nitrogen atmosphere. Ultrafine β-
The SiC powder + C (1 to 10 wt%) is sintered in an argon or nitrogen atmosphere. Or ultrafine β-SiC powder +
Si (1 to 10 wt%) is sintered in an argon or nitrogen atmosphere. The sintering conditions are as described above.
【００２５】ただし、超微粒β−ＳｉＣ粉末＋Ｃをアル
ゴン雰囲気中で焼結する場合は、ＳｉＣ粉末：Ｃ＝１：
５〜１０の混合粉末を作り、１時間アルゴン雰囲気中で
その粉末を２２００℃で処理し、ＳｉＣをβからαに構
造変換させ、その粉末を大気中で５００〜８００℃で空
気酸化させ、粉末中のＣを酸化させた粉末を出発材料と
して用いる。However, when sintering ultrafine β-SiC powder + C in an argon atmosphere, SiC powder: C = 1:
A mixed powder of 5 to 10 is prepared, and the powder is treated at 2200 ° C. in an argon atmosphere for 1 hour to convert the structure of SiC from β to α, and the powder is air-oxidized in air at 500 to 800 ° C. The powder obtained by oxidizing C therein is used as a starting material.
【００２６】Ｐ／Ｎ型焼結体のリード線の接合は、焼結
体に対して銅製のリード線を接合する必要がある。この
ため、Ｐ／Ｎ型焼結体のＰ及びＮ型それぞれの側に銅線
を下記要領に従ってろう付けする。For joining the lead wire of the P / N type sintered body, it is necessary to join a copper lead wire to the sintered body. For this purpose, a copper wire is brazed to each of the P and N type sides of the P / N type sintered body according to the following procedure.
【００２７】ＰないしＮ側とリード線の間にＴｉ＋Ｃｒ
（１〜３０ｗｔ％）系ろう材を挿入して、真空中で６０
０〜１０００℃の温度で１０ｋｇｆ〜１００ｋｇｆまで
のホットプレスを行い接合を行う。Ti + Cr between the P or N side and the lead wire
(1-30 wt%)-based brazing material is inserted, and the
A hot press of 10 kgf to 100 kgf is performed at a temperature of 0 to 1000 ° C. to perform joining.
【００２８】[0028]
【発明の効果】本発明のＳｉＣ（Ｐ型）／ＳｉＣ（Ｎ
型）等のセラミックス製熱電変換素子を原子炉（例え
ば、８５０℃以上の熱源となる原子炉炉心の周囲、高温
ガス炉、軽水炉、宇宙用原子炉等の炉心の周囲）の圧力
容器内及び高温配管に配置することにより、放射線損傷
を受けることなく高効率の熱電変換発電が長時間可能と
なる。According to the present invention, SiC (P type) / SiC (N
The thermoelectric conversion element made of ceramics, such as a mold, is placed in a pressure vessel of a reactor (for example, around a reactor core serving as a heat source of 850 ° C. or higher, around a core of a high-temperature gas reactor, a light water reactor, a space reactor, etc.) and at a high temperature. By arranging it in a pipe, high-efficiency thermoelectric conversion power generation can be performed for a long time without radiation damage.
【００２９】また、一般熱電としては、酸化雰囲気のボ
イラー容器の内外、家庭内でのヒーター等の熱源の周り
に配置するだけで発電や温度センサー等での利用が可能
となる。また、逆に本発明の熱電変換素子に電気を流す
ことによる熱電冷却素子として冷熱媒の冷却に利用する
ことも可能である。Further, as general thermoelectric, it is possible to use it for power generation, temperature sensor and the like simply by arranging it inside and outside the boiler vessel in an oxidizing atmosphere and around a heat source such as a heater in a home. Conversely, it is also possible to utilize the thermoelectric conversion element of the present invention as a thermoelectric cooling element for cooling a cooling medium by flowing electricity.
【図１】 各種混合粉末の焼結温度、電気抵抗及びＰ／
Ｎ型特性が示されている。Fig. 1 Sintering temperature, electric resistance and P /
N-type characteristics are shown.
【図２】 Ｐ型熱電変換素子における混合粉末中のボロ
ンカーバイトの添加量、焼結温度及び焼結体の電気抵抗
が示されている。FIG. 2 shows the addition amount of boron carbide in a mixed powder, a sintering temperature, and an electric resistance of a sintered body in a P-type thermoelectric conversion element.
【図３】 Ｎ型熱変換素子の高温における電気抵抗の変
化と温度との関係が示されている。FIG. 3 shows a relationship between a change in electric resistance of an N-type heat conversion element at a high temperature and a temperature.
【図４】 製作したＳｉＣ（Ｎ型）／Ｂ４Ｃ（Ｐ型）の
Ｐ／Ｎ型熱電変換素子の高温における起電力特性が示さ
れている。FIG. 4 shows an electromotive force characteristic of a manufactured SiC (N-type) / B4C (P-type) P / N-type thermoelectric conversion element at a high temperature.
Claims (6)
高効率で熱−電気変換できる熱電変換素子。1. In a high temperature and high radiation place such as a nuclear reactor,
Thermoelectric conversion element that can perform thermo-electric conversion with high efficiency.
でかつ起電力が数ｍＶ以上の耐熱性セラミックス材で製
作される請求項１に記載の熱電変換素子。2. The thermoelectric conversion element according to claim 1, wherein the thermoelectric conversion element is made of a heat-resistant ceramic material having an electric resistance of 10 ohm cm or less and an electromotive force of several mV or more.
い請求項３記載の熱電変換素子。3. The thermoelectric conversion element according to claim 3, wherein the thermoelectric conversion element is porous and has a low thermal conductivity and a high coefficient of performance Z.
ｗｔ％）をアルゴン又は窒素ガス雰囲気中で焼結するこ
とによりＰ型熱電変換素子を製造する方法。4. SiC + boron carbide (1 to 100
(wt%) in an argon or nitrogen gas atmosphere to produce a P-type thermoelectric conversion element.
（１〜１０ｗｔ％）をアルゴン雰囲気又は窒素ガス雰囲
気中で焼結することによりＮ型熱電変換素子を製造する
方法。5. SiC + C (1-10 wt%) or Si
(1 to 10 wt%) in an argon atmosphere or a nitrogen gas atmosphere to manufacture an N-type thermoelectric conversion element.
リード線間とを接合する方法。6. A method for joining a thermoelectric conversion element and a lead wire using a Ti-based brazing material.
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| JP11663898A JP3565544B2 (en) | 1998-04-27 | 1998-04-27 | Method for manufacturing ceramic thermoelectric conversion element used in high temperature and high radiation locations |
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|---|---|---|---|
| JP11663898A JP3565544B2 (en) | 1998-04-27 | 1998-04-27 | Method for manufacturing ceramic thermoelectric conversion element used in high temperature and high radiation locations |
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