JPH0435071A - Tehrmoelectric thin film and manufacture thereof - Google Patents
Tehrmoelectric thin film and manufacture thereofInfo
- Publication number
- JPH0435071A JPH0435071A JP2142814A JP14281490A JPH0435071A JP H0435071 A JPH0435071 A JP H0435071A JP 2142814 A JP2142814 A JP 2142814A JP 14281490 A JP14281490 A JP 14281490A JP H0435071 A JPH0435071 A JP H0435071A
- Authority
- JP
- Japan
- Prior art keywords
- iron
- thin film
- silicon
- thermoelectric thin
- ratio
- 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
- 239000010409 thin film Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 229910021417 amorphous silicon Inorganic materials 0.000 claims abstract description 6
- JRACIMOSEUMYIP-UHFFFAOYSA-N bis($l^{2}-silanylidene)iron Chemical compound [Si]=[Fe]=[Si] JRACIMOSEUMYIP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 10
- 229910000676 Si alloy Inorganic materials 0.000 claims description 3
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 2
- -1 oxygen ions Chemical class 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000010894 electron beam technology Methods 0.000 abstract description 6
- 239000010408 film Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 abstract 2
- 229910045601 alloy Inorganic materials 0.000 abstract 2
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000000097 high energy electron diffraction Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は熱起電力の大きい熱電薄膜及びその製造法に関
する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a thermoelectric thin film with a large thermoelectromotive force and a method for manufacturing the same.
（従来の技術及びその問題点）
β−鉄ジシリサイド粒子から構成される熱電材料は、種
々の排熱エネルギーがら電力を有効に回収するための材
料として注目されている。このβ鉄ジシリサイド粒子か
らなる熱電材料は、例えば電気学会技術報告（■部）第
２７５号（１９８８）に記載されているように、一般に
はα−鉄ジシリサイド粒子を成形焼結し、ついでアニー
リングして、α相をβ相に転換させることによって調製
される。このβ−鉄ジシリサイドからなる熱電材料の熱
電起電力（ゼーベック係数Ｓ）は高くとも０．５ ｍＶ
／ Ｋである。熱電材料を工業的に使用可能にするた
めには、その熱起電力を高めることが強く要望されてい
る。(Prior Art and its Problems) Thermoelectric materials composed of β-iron disilicide particles are attracting attention as materials for effectively recovering electric power from various types of waste heat energy. Thermoelectric materials made of β-iron disilicide particles are generally produced by molding and sintering α-iron disilicide particles and then annealing them, as described in, for example, IEEJ Technical Report (Part ■) No. 275 (1988). It is prepared by converting the α phase into the β phase. The thermoelectric electromotive force (Seebeck coefficient S) of this thermoelectric material made of β-iron disilicide is at most 0.5 mV.
/ K. In order to make thermoelectric materials industrially usable, it is strongly desired to increase their thermoelectromotive force.
（問題点を解決するための技術的手段）本発明は公知の
β−鉄ジシリサイド粒子からなる熱電材料に比較して高
い熱起電力を有する熱電薄膜及びその製造法を提供する
。(Technical Means for Solving the Problems) The present invention provides a thermoelectric thin film having a higher thermoelectromotive force than known thermoelectric materials made of β-iron disilicide particles, and a method for manufacturing the same.
本発明によれば、β−鉄ジシリサイド粒子と非晶質酸化
ケイ素との集合体からなる熱電薄膜が捉供される。According to the present invention, a thermoelectric thin film comprising an aggregate of β-iron disilicide particles and amorphous silicon oxide is provided.
さらに、本発明によれば、鉄原子に対するケイ素原子の
割合（以下ｒｓｉ／Ｆｅ比」ということがある。）が、
鉄ジシリサイドのケイ素原子の化学当量を超えている鉄
とケイ素との合金を、酸素イオンの存在下に蒸発させて
基板上に蒸着させ、ついでアニーリングするごとによっ
て、上記熱電薄膜を製造する方法が提供される。Furthermore, according to the present invention, the ratio of silicon atoms to iron atoms (hereinafter sometimes referred to as rsi/Fe ratio) is
A method is provided for producing the above-mentioned thermoelectric thin film by evaporating an alloy of iron and silicon in excess of the chemical equivalent of the silicon atoms of iron disilicide onto a substrate in the presence of oxygen ions, followed by annealing. be done.
本発明の熱電薄膜を構成する集合体の一方の成分である
β−鉄レジシリサイド粒子粒径は一般に５００Å以下で
ある。集合体の他方の成分である非晶質酸化ケイ素は二
酸化ケイ素及び−酸化ケイ素の両者を包含する。本明細
書において、「非晶質」とは、Ｘ線回折において明瞭な
ピークが観察されないことを言う。The particle diameter of β-iron resilicide particles, which is one component of the aggregate constituting the thermoelectric thin film of the present invention, is generally 500 Å or less. The other component of the assemblage, amorphous silicon oxide, includes both silicon dioxide and -silicon oxide. As used herein, "amorphous" means that no clear peak is observed in X-ray diffraction.
第１図及び第２図は、それぞれ、後述する実施例１で調
製された熱電薄膜（Ｓｉ／Ｆｅ比−３）のＸ線回折スペ
クトル及び赤外線吸収スペクトルである。第１図を参照
すると、本発明の熱電薄膜には、２θ−３０° （２２
０）及び５０° （４２２）にβ−鉄ジシリサイドの微
粒子に基づく回折が観察される。また、第２図を参照す
ると、本発明の熱電薄膜には、１１００ｃｒ＋ｒ’に５
ｉ−０−Ｓｉ結合に基づく吸収が、８００ｃｍ’にＳｉ
Ｏ□に基づく吸収が、さらに４３０ｃｎｒ’にβ−Ｆｅ
Ｓｉｚに基づく吸収がそれぞれ観察される。FIG. 1 and FIG. 2 are an X-ray diffraction spectrum and an infrared absorption spectrum, respectively, of a thermoelectric thin film (Si/Fe ratio -3) prepared in Example 1, which will be described later. Referring to FIG. 1, the thermoelectric thin film of the present invention has 2θ-30° (22
Diffraction based on fine particles of β-iron disilicide is observed at 0) and 50° (422). Also, referring to FIG. 2, the thermoelectric thin film of the present invention has a
Absorption based on the i-0-Si bond occurs at 800 cm'
The absorption based on O□ is further
Absorption based on Siz is observed respectively.
第３図は同じく本発明の実施例１で調製された熱電薄膜
（Ｓｉ／Ｆｅ比−３）の透過型電子顕微鏡像である。第
３図かられかるように、本発明の熱電薄膜は、β−鉄レ
ジシリサイド粒子図中の黒いスポット）が非晶質の酸化
ケイ素中に分散した集合体から構成されている。FIG. 3 is a transmission electron microscope image of a thermoelectric thin film (Si/Fe ratio -3) also prepared in Example 1 of the present invention. As can be seen from FIG. 3, the thermoelectric thin film of the present invention is composed of an aggregate of β-iron resilicide particles (black spots in the diagram) dispersed in amorphous silicon oxide.
本発明の熱電薄膜を構成する集合体におけるＳｉ／Ｆｅ
肚がβ−鉄ジシリサイドの化学当量より大であることが
、高い熱起電力を得るうえて重要である。上記Ｓｉ／Ｆ
ｅ比は２．５以上、特に３以上であることが好ましい。Si/Fe in the aggregate constituting the thermoelectric thin film of the present invention
It is important to have a higher chemical equivalent than the β-iron disilicide in order to obtain a high thermoelectromotive force. Above Si/F
The e ratio is preferably 2.5 or more, particularly 3 or more.
集合体におけるＳｉ／Ｐｅ比の−１−限については特別
の制限はないが、この比が過度に高（なると結果として
集合体中のβ−鉄ジシリサイドの割合が低下し、熱起電
力が低下するので、一般にＳｉ／Ｆｅ比の上限ば５であ
る。There is no particular restriction on the -1 limit of the Si/Pe ratio in the aggregate, but if this ratio is excessively high (as a result, the proportion of β-iron disilicide in the aggregate decreases, and the thermoelectromotive force decreases). Therefore, the upper limit of the Si/Fe ratio is generally 5.
熱電薄膜の厚さについても特別の制限はないが、一般に
は０．１〜ＩＯμｍである。There is no particular limit to the thickness of the thermoelectric thin film, but it is generally 0.1 to IO μm.
つぎに、本発明の熱電薄膜の製造法を図面を参照して説
明する。Next, a method for manufacturing a thermoelectric thin film according to the present invention will be explained with reference to the drawings.
第４図は、本発明の熱電薄膜の製造法に採用される装置
の一例の概略図である。FIG. 4 is a schematic diagram of an example of an apparatus employed in the thermoelectric thin film manufacturing method of the present invention.
反応室１ば開口２を有する隔壁３によって上部室４及び
下部室５とに区分けされている。下部室５の側壁には排
気管６か貫通して設けられ、図示しない減圧装置に連結
されている。熱電薄膜の調製時には反応室１は高度の真
空、例えば１×１０− ’ ｔｏｒｒに保持される。The reaction chamber 1 is divided into an upper chamber 4 and a lower chamber 5 by a partition wall 3 having an opening 2 . An exhaust pipe 6 is provided penetrating the side wall of the lower chamber 5 and is connected to a pressure reducing device (not shown). During the preparation of the thermoelectric thin film, the reaction chamber 1 is maintained at a high degree of vacuum, for example 1 x 10-' torr.
下部室５には電子ビーム発生ガン７が装着されており、
発生ガン７からの電子ビームは開口２を通って、隔壁３
に保持されているＳｉ／Ｆｅ比が２より大きい鉄とケイ
素の合金インゴット８の表面に照射され、この照射によ
って鉄及びケイ素の蒸気が発生する。An electron beam generating gun 7 is installed in the lower chamber 5.
The electron beam from the generating gun 7 passes through the aperture 2 and reaches the partition wall 3.
The surface of the iron-silicon alloy ingot 8 having a Si/Fe ratio of greater than 2 is irradiated, and iron and silicon vapor is generated by this irradiation.
」二部室４の中央側部にはイオンクラスタ−ビム発生器
９が装着されており、ボンへ１０から流量計１１を介し
て導管１２によって供給される酸素ガスのイオンビーム
を発生ずる。An ion cluster-beam generator 9 is mounted on the central side of the two-part chamber 4 and generates an ion beam of oxygen gas which is supplied by a conduit 12 from a bomb 10 via a flow meter 11.
鉄に比較して酸化されやすいケイ素蒸気とイオン化され
た酸素とが反応して、非晶質酸化ケイ素が生成し、鉄と
共に、ヒーター１３によって２００〜６００ ”Ｃに加
熱された基板１４上に膜状に堆積する。基板１４として
は、各種のセラミック板、石英板及びケイ素板を使用す
ることができる。Silicon vapor, which is more easily oxidized than iron, reacts with ionized oxygen to produce amorphous silicon oxide, which forms a film along with iron on the substrate 14 heated to 200-600''C by the heater 13. As the substrate 14, various ceramic plates, quartz plates, and silicon plates can be used.
堆積膜が所望の厚さになるまで上記の操作を継続した後
に、電子ビーム及び酸素イオンビームの発生を停止する
。ついで、真空下あるいはアルゴン、窒素などの不活性
ガス流通下にヒーター１３によって堆積膜を７５０〜９
００°Ｃの温度範囲に保持するアニーリングを行って、
鉄ジシリサイドの結晶をα相からβ相に転換して、本発
明の熱電薄膜が得られる。After continuing the above operation until the deposited film reaches a desired thickness, the generation of the electron beam and oxygen ion beam is stopped. Next, the deposited film is heated to 750 to 900 nm using a heater 13 under vacuum or under a flow of inert gas such as argon or nitrogen.
Annealing is performed at a temperature range of 00°C.
The thermoelectric thin film of the present invention can be obtained by converting iron disilicide crystals from α phase to β phase.
（実施例）
以下に実施例を示す。実施例において、熱電薄膜は第４
図に示す装置を使用して調製した。(Example) Examples are shown below. In embodiments, the thermoelectric thin film is the fourth
Prepared using the equipment shown in the figure.
実施例１ 下記反応条件で熱電薄膜を製造した。Example 1 A thermoelectric thin film was manufactured under the following reaction conditions.
反応室の圧力 Ｉ Ｘ １０−’Ｔｏｒｒ原料中
のＳｉ／Ｆｃ比 ２．０
膜堆積速度 ０．７２μｍ／ｈ」１記操作を継
続して厚さ６０００人の堆積膜を形成させた後に、アル
ゴンガス流通下に８００°Ｃで４時間アニーリングして
、熱電薄膜を調製した。Pressure in reaction chamber: I A thermoelectric thin film was prepared by annealing at 800°C for 4 hours under gas flow.
この薄膜中のＳｉ／Ｆｅ比を電子線マイクロアナライザ
ーで測定したところ、３．０であった。 得られた薄膜
のＸ線回折スペクトル及び赤外線スペクトルを、それぞ
れ、第１図及び第２図に示す。また、］二二記膜の高エ
ネルギー電子線回折図を第３図に示す。The Si/Fe ratio in this thin film was measured with an electron beam microanalyzer and was found to be 3.0. The X-ray diffraction spectrum and infrared spectrum of the obtained thin film are shown in FIGS. 1 and 2, respectively. Furthermore, a high-energy electron diffraction pattern of the XXII film is shown in FIG.
実施例２
原料中のＳｉ／Ｆｃ比を３．０に変えた以外は実施例１
を繰り返した。得れた熱電薄膜のＳｉ／Ｆｅ比を実施例
１と同様の方法で測定したとこと、３．８であった。Example 2 Example 1 except that the Si/Fc ratio in the raw material was changed to 3.0.
repeated. The Si/Fe ratio of the obtained thermoelectric thin film was measured in the same manner as in Example 1 and was found to be 3.8.
実施例１及び２で得られた熱電薄膜の熱起電力第１図及
び第２図は、それぞれ、本発明の熱電Ｆ７膜のＸ線回折
スペクトル及び赤外線吸収スペクＩ・ルであり、第３図
は本発明の熱電薄膜の粒子構造を示す図である。The thermoelectromotive forces of the thermoelectric thin films obtained in Examples 1 and 2 are shown in FIGS. 1 and 2, respectively, and the X-ray diffraction spectrum and infrared absorption spectrum of the thermoelectric F7 film of the present invention are shown in FIG. FIG. 2 is a diagram showing the particle structure of the thermoelectric thin film of the present invention.
第４図は本発明の熱電薄膜の製造に使用される装置の一
例の概略図である。FIG. 4 is a schematic diagram of an example of an apparatus used for manufacturing the thermoelectric thin film of the present invention.
第５図は実施例で得られた熱電薄膜の熱起電力を示す図
である。FIG. 5 is a diagram showing the thermoelectromotive force of the thermoelectric thin film obtained in the example.
１・・・反応室
７・・・電子ビーム発生ガン
８・・・鉄ジシリサイドのインゴット
９・・・イオンクラスタービーム発生器１３・・・ヒー
タ
１４・・・基板
２０ （ｌｅり・）
ンルミ −ｆ、ｙ （ｔｔｎ−’ ）３０λ1...Reaction chamber 7...Electron beam generating gun 8...Iron disilicide ingot 9...Ion cluster beam generator 13...Heater 14...Substrate 20 ,y (ttn-')30λ
Claims (3)
集合体からなる熱電薄膜。(1) A thermoelectric thin film consisting of an aggregate of β-iron disilicide particles and amorphous silicon oxide.
リサイドのケイ素原子の化学当量を超えている集合体か
らなる、特許請求の範囲第１項に記載の熱電薄膜。(2) The thermoelectric thin film according to claim 1, comprising an aggregate in which the ratio of silicon atoms to iron atoms exceeds the chemical equivalent of silicon atoms in β-iron disilicide.
ドのケイ素原子の化学当量を超えている鉄とケイ素との
合金を、酸素イオンの存在下に蒸発させて基板上に蒸着
させ、ついでアニーリングすることを特徴とする、特許
請求の範囲第１項に記載の熱電薄膜の製造法。(3) An alloy of iron and silicon in which the ratio of silicon atoms to iron atoms exceeds the chemical equivalent of silicon atoms in iron disilicide is evaporated onto a substrate in the presence of oxygen ions, and then annealed. A method for producing a thermoelectric thin film according to claim 1, characterized by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2142814A JPH0435071A (en) | 1990-05-31 | 1990-05-31 | Tehrmoelectric thin film and manufacture thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2142814A JPH0435071A (en) | 1990-05-31 | 1990-05-31 | Tehrmoelectric thin film and manufacture thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0435071A true JPH0435071A (en) | 1992-02-05 |
Family
ID=15324251
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2142814A Pending JPH0435071A (en) | 1990-05-31 | 1990-05-31 | Tehrmoelectric thin film and manufacture thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0435071A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5547598A (en) * | 1993-08-04 | 1996-08-20 | Technova, Inc. | Thermoelectric semiconductor material |
-
1990
- 1990-05-31 JP JP2142814A patent/JPH0435071A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5547598A (en) * | 1993-08-04 | 1996-08-20 | Technova, Inc. | Thermoelectric semiconductor material |
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