JPS63176393A - Production of aluminum nitride thin film - Google Patents
Production of aluminum nitride thin filmInfo
- Publication number
- JPS63176393A JPS63176393A JP62008481A JP848187A JPS63176393A JP S63176393 A JPS63176393 A JP S63176393A JP 62008481 A JP62008481 A JP 62008481A JP 848187 A JP848187 A JP 848187A JP S63176393 A JPS63176393 A JP S63176393A
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- aluminum
- aluminum nitride
- nitride thin
- nitrogen
- 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 25
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000000758 substrate Substances 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000005284 excitation Effects 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000010891 electric arc Methods 0.000 abstract description 2
- -1 nitrogen-containing compound Chemical class 0.000 abstract 2
- 238000000034 method Methods 0.000 description 7
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005162 X-ray Laue diffraction Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/10—Heating of the reaction chamber or the substrate
- C30B25/105—Heating of the reaction chamber or the substrate by irradiation or electric discharge
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/38—Nitrides
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は低温で結晶性、電気的特性の良い結晶化窒化ア
ルミニウム薄膜を製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for producing a crystallized aluminum nitride thin film having good crystallinity and electrical properties at low temperatures.
従来の技術
基板材料、表面弾性波素子用材料、光学素子用材料とし
てすぐれた特性を持つ窒化アルミニウム薄膜は真空蒸着
、スパッタリング、あるいはＣｖＤ等の方法で作製され
ている。Conventional technology Aluminum nitride thin films, which have excellent properties as substrate materials, surface acoustic wave device materials, and optical device materials, are produced by methods such as vacuum evaporation, sputtering, or CVD.
発明が解決しようとする問題点
いずれの薄膜形成法においても、アルミニウムと窒素の
反応により窒化アルミニウム薄膜が形成されるわけであ
るが、結晶化窒化アルミニウム薄膜の作製のためには基
板温度として８００℃〜１０００℃以上の温度が必要で
あり、プロセス上大きな欠点となっている。また、基板
の熱エネルギーのみでは原料の分解が不十分であったり
、基板表面での原子のマイグレイジョンが十分に行われ
ないため結晶性の点で満足のゆく薄膜が得られていると
は言いがたいのが現状である。Problems to be Solved by the Invention In both thin film formation methods, an aluminum nitride thin film is formed by a reaction between aluminum and nitrogen, but in order to fabricate a crystallized aluminum nitride thin film, the substrate temperature must be 800°C. A temperature of ~1000°C or higher is required, which is a major drawback in terms of the process. In addition, it is difficult to obtain a thin film that is satisfactory in terms of crystallinity because the thermal energy of the substrate alone is insufficient to decompose the raw materials or migration of atoms on the substrate surface is not sufficient. The current situation is difficult to say.
本発明は、結晶性の良い不純物の少ない窒化アルミニウ
ム薄膜を低温で得るための方法を提供することを目的と
する。An object of the present invention is to provide a method for obtaining an aluminum nitride thin film with good crystallinity and few impurities at a low temperature.
問題点を解決するための手段
アルミニウム、またはアルミニウムを含む化合物の励起
種と、窒素、または窒素を含む化合物の励起種と、解離
水素とを反応させることで基板上に低温で結晶性の良い
化合物薄膜を得る。Means for solving the problem A compound with good crystallinity is formed on a substrate at a low temperature by reacting an excited species of aluminum or a compound containing aluminum with nitrogen or an excited species of a compound containing nitrogen and dissociated hydrogen. Obtain a thin film.
作用
励起種を用いた反応は基本的に活性化エネルギ−を持た
ない反応なので低温で窒化アルミニウムの合成が可能に
なる。さらに、解離水素の高い内部エネルギー（４３１
ｋＪ／ｍｏｌ ）により基板上での反応、マイグレーシ
ョン、表面不純物の除去が促進され、さらに水素原子に
よるダングリングボンドのパシベーション効果により、
低温で結晶性、電気特性の優れた薄膜形成が可能になる
。Since reactions using active excited species basically have no activation energy, it is possible to synthesize aluminum nitride at low temperatures. Furthermore, the high internal energy of dissociated hydrogen (431
kJ/mol ) promotes reaction, migration, and removal of surface impurities on the substrate, and furthermore, the passivation effect of dangling bonds by hydrogen atoms
It becomes possible to form thin films with excellent crystallinity and electrical properties at low temperatures.
実施例
以下、図面を参照して、実施例にもとすき本発明の詳細
な説明する。EXAMPLES Hereinafter, the present invention will be described in detail by way of examples with reference to the drawings.
まず、本薄膜製造法による薄膜製造装置の構成を第１図
に示す。図中１はりアクタ−１２はグラファイト製サセ
プタ、３は基板である。グラファイト製サセプタを高周
波誘導加熱により加熱し、熱伝導により基板を加熱した
。各ボンベからの原料ガスは、それぞれ４１〜４３の発
生部で活性化された。活性化の方法としては、本実施例
ではマイクロ波プラズマを用いたが、この他、アーク放
電、レーザー励起、紫外光照射、ＥＣＲプラズマ等を用
いてもよい。ヘリウムで希釈したトリメチルアルミニウ
ム（ＴＭＡ）をボンベ５１から、アンモニアガスをボン
ベ５２から、そして水素ガスをボンベ５３から供給した
。それぞれ流量はマスフローコントロラー６１を用いて
調節した。基板には（０００１）サファイアを用いた。First, FIG. 1 shows the configuration of a thin film manufacturing apparatus using the present thin film manufacturing method. In the figure, 1 beam actor 12 is a graphite susceptor, and 3 is a substrate. A graphite susceptor was heated by high-frequency induction heating, and the substrate was heated by thermal conduction. The raw material gas from each cylinder was activated at generation points 41 to 43, respectively. Although microwave plasma was used in this embodiment as an activation method, other methods such as arc discharge, laser excitation, ultraviolet light irradiation, and ECR plasma may also be used. Trimethylaluminum (TMA) diluted with helium was supplied from a cylinder 51, ammonia gas from a cylinder 52, and hydrogen gas from a cylinder 53. Each flow rate was adjusted using a mass flow controller 61. (0001) sapphire was used for the substrate.
ＴＭＡおよびアンモニアは約１０ ’ｍｏｌ／ｓｉｎの
割合で供給した。TMA and ammonia were supplied at a rate of about 10'mol/sin.
基板温度３００℃以上で結晶化した窒化アルミニウムの
薄膜が得られた。表面は光学的に平面で３００℃で成長
した薄膜はＸ線回折パターンにおいてＣ軸に垂直な面の
反射のみが非常に強く現れた。A thin film of aluminum nitride crystallized at a substrate temperature of 300° C. or higher was obtained. The surface of the thin film was optically flat and was grown at 300° C. In the X-ray diffraction pattern, only the reflection on the plane perpendicular to the C axis appeared very strongly.
ラウェ写真を撮影したところ、第２図に示すような回折
パターンが得られた。Ｘ線のビーム径は約２ＩＩ１１で
あり、膜面に垂直に入射した。約５Ｘ５ｍｍの窒化アル
ミニウム薄膜中ではいずれの位置においても第２図に示
すような回折パターンが得られたことから単結晶薄膜が
得られたことがわかる。この薄膜の電気抵抗を測定した
ところ１０”Ω・Ｃｌ１１と極めて高く、純度が高く欠
陥の少ない窒化アルミニウム薄膜が基板温度わずか３０
０℃で形成されたことがわかる。When a Laue photograph was taken, a diffraction pattern as shown in FIG. 2 was obtained. The beam diameter of the X-rays was approximately 2II11 and was incident perpendicularly to the film surface. It can be seen that a single crystal thin film was obtained since a diffraction pattern as shown in FIG. 2 was obtained at any position in the approximately 5×5 mm aluminum nitride thin film. When the electrical resistance of this thin film was measured, it was extremely high at 10"Ω・Cl11, and the aluminum nitride thin film with high purity and few defects was found to have a substrate temperature of only 30%.
It can be seen that it was formed at 0°C.
また、第１１の構成も本発明の主旨を損なわない範囲に
おいて各種の変形が可能であることは明らかである。そ
して、本発明の主旨を損なわない範囲において本発明は
スパッタリング法、真空蒸着法等にも応用される。Further, it is clear that various modifications can be made to the eleventh configuration without departing from the spirit of the present invention. The present invention may also be applied to sputtering methods, vacuum evaporation methods, etc., within the scope of not detracting from the gist of the present invention.
発明の効果
以上の説明から明らかな様に、本発明による薄膜形成法
では、解離水素原子の持つ大きな内部エネルギーが薄膜
形成に用いられるため低い基板温度で窒化アルミニウム
薄膜の形成が可能になる。Effects of the Invention As is clear from the above explanation, in the thin film forming method according to the present invention, the large internal energy of dissociated hydrogen atoms is used for thin film formation, so that it is possible to form an aluminum nitride thin film at a low substrate temperature.
第１図は本発明の実施例で用いた試料作製装置の模式図
、第２図は薄膜のラウェ写真の転写図である。
１・・・リアクタ、２・・・サセプタ、３・・・基板、
４１〜４３・・・発生部、５１・・・ＴＭＡ、５２・・
・ＮＨ３，５３・・・Ｈ２，６１・・・マスフローコン
トローラー、７１・・・高周波コイル、８１・・・排気
口。
代理人の氏名 弁理士 中尾敏男 ほか１名＝
” 第１図
第２図FIG. 1 is a schematic diagram of a sample preparation apparatus used in an example of the present invention, and FIG. 2 is a transfer diagram of a Laue photograph of a thin film. 1...Reactor, 2...Susceptor, 3...Substrate,
41-43... Generation part, 51... TMA, 52...
・NH3,53...H2,61...Mass flow controller, 71...High frequency coil, 81...Exhaust port. Name of agent: Patent attorney Toshio Nakao and one other person = ” Figure 1 Figure 2
Claims (1)
種と、窒素、または窒素を含む化合物の励起種と、解離
水素とを反応させることにより基板上に窒化アルミニウ
ム薄膜を作製することを特徴とする窒化アルミニウム薄
膜の製造方法。An aluminum nitride thin film is produced on a substrate by reacting an excited species of aluminum or a compound containing aluminum, nitrogen or an excited species of a compound containing nitrogen, and dissociated hydrogen. Production method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62008481A JPS63176393A (en) | 1987-01-16 | 1987-01-16 | Production of aluminum nitride thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62008481A JPS63176393A (en) | 1987-01-16 | 1987-01-16 | Production of aluminum nitride thin film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63176393A true JPS63176393A (en) | 1988-07-20 |
Family
ID=11694298
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62008481A Pending JPS63176393A (en) | 1987-01-16 | 1987-01-16 | Production of aluminum nitride thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63176393A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02141496A (en) * | 1988-11-22 | 1990-05-30 | Alps Electric Co Ltd | Method for synthesizing aluminum nitride |
| JPH04136173A (en) * | 1990-09-25 | 1992-05-11 | Alps Electric Co Ltd | Method for depositing synthetic film |
| JP2008019140A (en) * | 2006-07-14 | 2008-01-31 | Ngk Insulators Ltd | METHOD FOR FORMING AlN SINGLE CRYSTAL FILM |
| JP2008159958A (en) * | 2006-12-26 | 2008-07-10 | Showa Denko Kk | Manufacturing method of group iii nitride semiconductor, manufacturing method of group iii nitride semiconductor light-emitting element, group iii nitride semiconductor light-emitting element and lamp |
| WO2009096270A1 (en) * | 2008-01-31 | 2009-08-06 | Canon Anelva Corporation | AlN HETEROEPITAXIAL CRYSTAL, METHOD FOR PRODUCING THE SAME, BASE SUBSTRATE FOR GROUP III NITRIDE FILM USING THE CRYSTAL, LIGHT-EMITTING DEVICE, SURFACE ACOUSTIC WAVE DEVICE, AND SPUTTERING APPARATUS |
-
1987
- 1987-01-16 JP JP62008481A patent/JPS63176393A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02141496A (en) * | 1988-11-22 | 1990-05-30 | Alps Electric Co Ltd | Method for synthesizing aluminum nitride |
| JPH04136173A (en) * | 1990-09-25 | 1992-05-11 | Alps Electric Co Ltd | Method for depositing synthetic film |
| JP2008019140A (en) * | 2006-07-14 | 2008-01-31 | Ngk Insulators Ltd | METHOD FOR FORMING AlN SINGLE CRYSTAL FILM |
| JP2008159958A (en) * | 2006-12-26 | 2008-07-10 | Showa Denko Kk | Manufacturing method of group iii nitride semiconductor, manufacturing method of group iii nitride semiconductor light-emitting element, group iii nitride semiconductor light-emitting element and lamp |
| WO2009096270A1 (en) * | 2008-01-31 | 2009-08-06 | Canon Anelva Corporation | AlN HETEROEPITAXIAL CRYSTAL, METHOD FOR PRODUCING THE SAME, BASE SUBSTRATE FOR GROUP III NITRIDE FILM USING THE CRYSTAL, LIGHT-EMITTING DEVICE, SURFACE ACOUSTIC WAVE DEVICE, AND SPUTTERING APPARATUS |
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