JPH01252786A - Method for synthesizng aluminum nitride film - Google Patents
Method for synthesizng aluminum nitride filmInfo
- Publication number
- JPH01252786A JPH01252786A JP7961588A JP7961588A JPH01252786A JP H01252786 A JPH01252786 A JP H01252786A JP 7961588 A JP7961588 A JP 7961588A JP 7961588 A JP7961588 A JP 7961588A JP H01252786 A JPH01252786 A JP H01252786A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- aluminum
- aluminum nitride
- nitride film
- 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
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims description 21
- 238000000034 method Methods 0.000 title claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 15
- 239000011888 foil Substances 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 30
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 30
- 230000002194 synthesizing effect Effects 0.000 claims description 7
- 230000005284 excitation Effects 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 15
- 238000000926 separation method Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000012159 carrier gas Substances 0.000 description 6
- 125000002524 organometallic group Chemical group 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000012050 conventional carrier Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
Landscapes
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
この発明は１機械部品用摺動部材或いは回路用基板など
に応用できる窒化アルミニウム膜の簡単かつ安全な合成
方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a simple and safe method for synthesizing an aluminum nitride film that can be applied to sliding members for mechanical parts, circuit boards, etc.
（従来の技術）
近年、窒化アルミニウムは高熱伝導性の他に高絶縁性、
高絶縁耐圧性、そして低誘電性などの電気的特性を兼ね
備えた材料として注目されている。(Conventional technology) In recent years, aluminum nitride has not only high thermal conductivity but also high insulation and
It is attracting attention as a material that has electrical properties such as high dielectric strength and low dielectricity.
そしてその窒化アルミニウム材料は、主として焼結体と
してよく使用されているが、さらに短小軽薄化の要求と
共に窒化アルミニウム膜も開発され。The aluminum nitride material is often used primarily as a sintered body, but aluminum nitride films have also been developed in response to demands for shorter, lighter, and thinner bodies.
回路用基板、機械用摺動部材に応用されている。It is applied to circuit boards and mechanical sliding parts.
従来の窒化アルミニウム膜の合成方法は、図面第５図に
示すように、励起装置４と加熱装置５とを備えた反応室
７に窒素源ガス供給装置１を接続し、前記反応室７とキ
ャリアガス供給装置２との間にアルミニウム系の有機金
属供給装置３を設け、前記反応室７と真空排気装置６を
接続した装置が用いられていた。In the conventional method for synthesizing an aluminum nitride film, as shown in FIG. 5, a nitrogen source gas supply device 1 is connected to a reaction chamber 7 equipped with an excitation device 4 and a heating device 5. An apparatus was used in which an aluminum-based organometallic supply device 3 was provided between the gas supply device 2 and the reaction chamber 7 and the evacuation device 6 were connected.
まず反応室７内の基体支持体９の上へ、例えはサファイ
アのような絶縁物である基体８を置き、窒素源ガス供給
装置１から５例えばアンモニアまたは窒素ガスを反応室
７へ供給し、また別系統であるキャリアガス供給袋Ｎ２
から、例えば水素キャリアガスをアルミニウム系の有機
金属供給装置３内に通し反応室７へ供給する。なお前記
窒素源ガスとキャリアガスを反応室７へ供給する時には
。First, a substrate 8, which is an insulating material such as sapphire, is placed on a substrate support 9 in a reaction chamber 7, and a nitrogen source gas supply device 5, such as ammonia or nitrogen gas, is supplied to the reaction chamber 7. Another system is carrier gas supply bag N2.
For example, hydrogen carrier gas is passed through the aluminum-based organometallic supply device 3 and supplied to the reaction chamber 7 . Note that when the nitrogen source gas and carrier gas are supplied to the reaction chamber 7.
反応室７内を、真空排気装置６によって減圧下に保たせ
る。前記窒素源ガスとアルミニウム系有機金属を含んだ
キャリアガスは、基体８の近傍で励起装置４によって励
起され、加熱装置５によって加熱された基体８上で化学
反応を起こし、この化学反応によって基体８上へ窒化ア
ルミニウムが合成されていた。The inside of the reaction chamber 7 is kept under reduced pressure by the vacuum evacuation device 6. The carrier gas containing the nitrogen source gas and the aluminum-based organic metal is excited by the excitation device 4 near the substrate 8 and causes a chemical reaction on the substrate 8 heated by the heating device 5. Aluminum nitride was synthesized on top.
（発明が解決しようとする問題点）
従来の窒素”源とアルミニウム系有機金属を用いた窒化
アルミニウム膜の合成方法には以下のような欠点、問題
があった。(Problems to be Solved by the Invention) The conventional method of synthesizing an aluminum nitride film using a nitrogen source and an aluminum-based organic metal has the following drawbacks and problems.
（１） アルミニウム系有機金属は空気中で容易に酸化
される性質があり多量に漏洩した場合には自然発火ある
いは爆発する場合もあった。従ってアルミニウム系有機
金属と空気が接触しないようなリークフリーの装置を必
要とした。そのリークフリー装置の一例として有機金属
の周辺をさらに容器でおおい、その容器中を窒素ガスで
充満しておくシステムも存在した。(1) Aluminum-based organic metals have the property of being easily oxidized in the air, and if a large amount leaks, spontaneous combustion or explosion may occur. Therefore, a leak-free device was required that would prevent air from coming into contact with the aluminum-based organic metal. As an example of such a leak-free device, there was also a system in which the area around the organic metal was further covered with a container, and the container was filled with nitrogen gas.
また同時にリーグチエツクも毎回性なわなければならず
、そのことはリークチエツクの手間がかかるだけではな
く、高感度なヘリウムリークディテクターと大気中の水
分による誤動作を防止するための高純度ヘリウ１１を必
要としていた。そしてそれらに対するコストも装置なみ
の金額か必要であった・
（２） アルミニウム系有機金属は、水と激しく反応し
、炭化水素ガスを発生し１発火する性質も持ち合わせて
いる。従って反応系内の水分は十分に除去させなければ
ならなかった。例えば水素ガスにて水分を除去する場合
は、流量５０ ｃｃ ／ ｗｉｎで１週間位とされてい
た。At the same time, a leak check must be performed every time, which not only takes time and effort, but also requires a highly sensitive helium leak detector and high-purity helium-11 to prevent malfunctions caused by moisture in the atmosphere. It was. And the costs for these were as high as the equipment. (2) Aluminum-based organic metals have the property of reacting violently with water, generating hydrocarbon gas, and igniting. Therefore, the water in the reaction system had to be sufficiently removed. For example, when removing moisture using hydrogen gas, the flow rate was 50 cc/win for about one week.
この発明は従来のものがもつ問題点を解消させるアルミ
ニウム系有機金属を用いることのない窒化アルミニウム
膜の合成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 synthesizing an aluminum nitride film that eliminates the problems of the conventional method and does not use an aluminum-based organic metal.
（問題点を解決するための手段）
この発明は、その目的を達成させるために次のような構
成としている。(Means for Solving the Problems) The present invention has the following configuration in order to achieve the object.
この発明の要旨とするところは、基体をアルミニウム箔
で包み、窒素系ガスの加熱励起によって、この基体上に
窒化アルミニウム膜を生成させることを特徴とする窒化
アルミニウム膜の合成方法にある。すなわち、この発明
は従来のキャリアガス供給装置及びアルミニウム系の有
機金属供給装置を除いて窒化アルミニウム膜を合成する
特徴を有している。The gist of the present invention is a method for synthesizing an aluminum nitride film, which is characterized in that the substrate is wrapped in aluminum foil and an aluminum nitride film is formed on the substrate by heating and excitation of a nitrogen-based gas. That is, the present invention has a feature of synthesizing an aluminum nitride film without using the conventional carrier gas supply device and aluminum-based organometallic supply device.
この発明を以下図面について詳説する。The invention will be explained in detail below with reference to the drawings.
アルミニウム源系統は第２図に示すように基体支持体９
上に脱離板１０を置き、その上にアルミニウム箔１１で
包んだ基体８を置く構造をとっている。The aluminum source system is connected to the base support 9 as shown in FIG.
The structure is such that a release plate 10 is placed on top, and a base 8 wrapped in aluminum foil 11 is placed on top of it.
一方、窒素源系統１例えば窒素ガスは窒素源ガス供給装
置１によって反応室７へ送られる。基体８を包んでいる
アルミニウム箔１１は、加熱装置５によってアルミニウ
ムの融点以上の例えば９００℃にて溶融する。脱離板１
０は基体支持体９と基体８が溶融したアルミニウムによ
って付着することを防止するために使用される。On the other hand, the nitrogen source system 1 , for example, nitrogen gas, is sent to the reaction chamber 7 by the nitrogen source gas supply device 1 . The aluminum foil 11 surrounding the base 8 is melted by the heating device 5 at a temperature higher than the melting point of aluminum, for example, 900°C. Detachment plate 1
0 is used to prevent substrate support 9 and substrate 8 from sticking together due to molten aluminum.
反応室７内で窒素源系統のガスは、励起装置４によって
励起され、溶融したアルミニウムと化学反応が生じる。In the reaction chamber 7, the gas of the nitrogen source system is excited by the excitation device 4, and a chemical reaction occurs with the molten aluminum.
この化学反応により基体８上へ窒化アルミニウム膜が合
成される。Through this chemical reaction, an aluminum nitride film is synthesized on the substrate 8.
（実施例］） 基体をアルミニウム箔で包む方法を第３図に示す。(Example]) FIG. 3 shows a method of wrapping the substrate with aluminum foil.
マイクロ波出力２５０Ｗ使用アルミニウム箔サイズ１９
Ｘ Ｌｌ ９ Ｘ ０ 、 Ｏ２５（ｍｍ）窒素ガ
ス流量 ７５３ＣＣＭ
圧力 ３５ ｍｍ Ｈｇ
基体 シリコンウェハー（５１１）面サイズＷ１５
Ｘ Ｌｌ ５ Ｘｔｏ、 ６ （＋１１０１）合成時間
３０分
脱離板 黒鉛シート
上記条件で行ったところ基板温度は光高温計で９００℃
を示した。Uses microwave output 250W Aluminum foil size 19
X Ll 9 X 0, O25 (mm) Nitrogen gas flow rate 753 CCM Pressure 35 mm Hg Substrate Silicon wafer (511) surface size W15
X Ll 5
showed that.
合成サンプルのＸ＠回折（回折角２０”−７５゛）を行
なったところ下記の表１のような結果を示した。When the synthesized sample was subjected to X@ diffraction (diffraction angle 20"-75"), the results were shown in Table 1 below.
表 １
（強度：Ｓ・・・強い２ｍ・・中間、Ｗ・・・弱い）観
察物質は窒化アルミニウム膜と同定できた。Table 1 (Strength: S...strong 2m...medium, W...weak) The observed substance could be identified as an aluminum nitride film.
（実施例２） 基体をアルミニウム箔で包む方法を第４図に示す。(Example 2) FIG. 4 shows a method of wrapping the substrate with aluminum foil.
マイクロ波出力２５０Ｗ使用アルミニウム箔サイＸｖ′
ｌ ４ ＸＬｌ ４ Ｘｔｏ 、 Ｏ２５（１１１１１
）窒素ガス流量１９ＳＣＣｉｌｌ水流ガス流、ｆｆｉ：
５６ＳＣＣＭ圧力 ３５ｍｍＨｇ
基体 窒化珪素針状結晶体
サイズ′Ｎ１０×Ｌ１０Ｘ七４ （ｎ＋ｎ＋）合成時間
２０分
脱離板 アルミナ板
上記の条件で合成を行ったところ基板温度は光高温計で
１０００℃を示した
合成サンプルのＸ線回折（回折角２０’−７５°）を行
ったところ下記の表２のような結果を示した。Aluminum foil size Xv' using microwave output 250W
l 4 XLl 4 Xto , O25 (11111
) Nitrogen gas flow rate 19 SCCill water gas flow, ffi:
56SCCM Pressure 35mmHg Substrate Silicon nitride needle crystal size 'N10 x L10 When the synthesized sample was subjected to X-ray diffraction (diffraction angle 20'-75°), the results shown in Table 2 below were shown.
表 ２
（強度：Ｓ・・・強い２ｍ・・・中間、Ｗ・・・弱い）
観察物質は窒化アルミニウム膜と同定できた。Table 2 (Strength: S...Strong 2m...Intermediate, W...Weak)
The observed substance was identified as aluminum nitride film.
（実施例３）
この発明で合成した窒化アルミニウム膜を８００℃の条
件下で使用される軸受けの摺動面へ使用した。(Example 3) The aluminum nitride film synthesized according to the present invention was used on the sliding surface of a bearing used at 800°C.
窒化アルミニウム膜が無い軸受については、１ケ月で損
耗し交換するのに対し、窒化アルミニウム膜を摺動面へ
使用した軸受については、２ケ月経過後も損耗の問題が
無く使用に供した。Bearings without aluminum nitride film were worn out after one month and had to be replaced, whereas bearings with aluminum nitride film on their sliding surfaces were used without any wear problems even after two months.
（発明の効果）
この発明によって以下のような優れた効果を得ることが
できる。(Effects of the Invention) The following excellent effects can be obtained by this invention.
■ 自然発火性のアルミニウム系有機金属を使用しなく
ても窒化アルミニウムの合成ができるから、安全に取扱
いができる。■ Aluminum nitride can be synthesized without using pyrophoric aluminum-based organic metals, so it can be handled safely.
■ 従来はリークチエツク及び水分除去の前段取時間に
約１０時間型していたのに対してこの発明方法を用いる
と完全に前段取時間を無くすことができるから、合成時
間の短縮ができる。(2) Conventionally, the pre-setup time for leak check and moisture removal required about 10 hours, but with the method of the present invention, the pre-setup time can be completely eliminated, so the synthesis time can be shortened.
■ リークディテクター、高純度ヘリウム、キャリアガ
ス供給装置、アルミニウム系の有機金属供給装置を使用
せず、さらに高価なアルミニウム系の有機金属原料の代
わりに超安値なアルミニウム箔を使用するため、安価に
合成ができる。■ Low-cost synthesis because it does not use a leak detector, high-purity helium, carrier gas supply device, or aluminum-based organometallic supply device, and uses ultra-cheap aluminum foil instead of the expensive aluminum-based organometallic raw material. I can do it.
第１図はこの発明の方法を実施する装置の概要説明図、
第２図は同基体周辺の詳細説明図、第３図は同実施例１
におけるシリコンウェハー基体をアルミニウム箔で包む
状態を示した説明図、第４図は同実施例２における窒化
珪素針状結晶体をアルミニウム箔で包む状態を示した説
明図、第５図は従来の方法を実施する装置の概要説明図
である。
１・・・窒素源ガス供給装置、２・・・キャリアガス供
給装置、３・・・アルミニウム系の有機金属供給装置、
４・・・励起装置、５・・・加熱装置、６・・・真空排
気装置、７・・・反応室、８・・・基体、９・・・基体
支持体、１０・・・脱離板、１１・・・アルミニウム箔
、
特許出願人 東京窯業株式会社
第 １ 図
第 ２ 図
第５図
／／、＋アルミニウム乃FIG. 1 is a schematic explanatory diagram of an apparatus for carrying out the method of this invention;
Figure 2 is a detailed explanatory diagram of the surroundings of the same base, and Figure 3 is Example 1 of the same.
FIG. 4 is an explanatory diagram showing the state in which the silicon wafer substrate is wrapped in aluminum foil in Example 2, FIG. 4 is an explanatory diagram showing the state in which the silicon nitride needle crystal body in Example 2 is wrapped in aluminum foil, and FIG. 1 is a schematic explanatory diagram of an apparatus for implementing 1... Nitrogen source gas supply device, 2... Carrier gas supply device, 3... Aluminum-based organometallic supply device,
4... Excitation device, 5... Heating device, 6... Evacuation device, 7... Reaction chamber, 8... Substrate, 9... Substrate support, 10... Desorption plate , 11... Aluminum foil, Patent applicant Tokyo Ceramics Co., Ltd. Figure 1 Figure 2 Figure 5 //, + Aluminum No
Claims (1)
励起によって、この基体８上に窒化アルミニウム膜を生
成させることを特徴とする窒化アルミニウム膜の合成方
法。A method for synthesizing an aluminum nitride film, which comprises wrapping a substrate 8 with an aluminum foil 11 and generating an aluminum nitride film on the substrate 8 by heating and excitation of a nitrogen-based gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7961588A JPH01252786A (en) | 1988-03-31 | 1988-03-31 | Method for synthesizng aluminum nitride film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7961588A JPH01252786A (en) | 1988-03-31 | 1988-03-31 | Method for synthesizng aluminum nitride film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01252786A true JPH01252786A (en) | 1989-10-09 |
Family
ID=13694959
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7961588A Pending JPH01252786A (en) | 1988-03-31 | 1988-03-31 | Method for synthesizng aluminum nitride film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01252786A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03264755A (en) * | 1990-03-14 | 1991-11-26 | Toyota Motor Corp | Aluminum alloy-made piston and manufacture thereof |
| US5294264A (en) * | 1990-04-20 | 1994-03-15 | Martin Marietta Energy Systems, Inc. | Method of nitriding refractory metal articles |
| JP2002268046A (en) * | 2001-03-13 | 2002-09-18 | Sumitomo Bakelite Co Ltd | Plastic substrate for display |
-
1988
- 1988-03-31 JP JP7961588A patent/JPH01252786A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03264755A (en) * | 1990-03-14 | 1991-11-26 | Toyota Motor Corp | Aluminum alloy-made piston and manufacture thereof |
| US5294264A (en) * | 1990-04-20 | 1994-03-15 | Martin Marietta Energy Systems, Inc. | Method of nitriding refractory metal articles |
| JP2002268046A (en) * | 2001-03-13 | 2002-09-18 | Sumitomo Bakelite Co Ltd | Plastic substrate for display |
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