JPH01319682A - Formation of aluminum nitride film - Google Patents
Formation of aluminum nitride filmInfo
- Publication number
- JPH01319682A JPH01319682A JP15174288A JP15174288A JPH01319682A JP H01319682 A JPH01319682 A JP H01319682A JP 15174288 A JP15174288 A JP 15174288A JP 15174288 A JP15174288 A JP 15174288A JP H01319682 A JPH01319682 A JP H01319682A
- Authority
- JP
- Japan
- Prior art keywords
- soln
- film
- base
- contg
- metal alkoxide
- 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 6
- 230000015572 biosynthetic process Effects 0.000 title description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 17
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 3
- 238000007598 dipping method Methods 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 2
- 239000002904 solvent Substances 0.000 abstract 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 abstract 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 abstract 1
- 229910001679 gibbsite Inorganic materials 0.000 abstract 1
- MYWQGROTKMBNKN-UHFFFAOYSA-N tributoxyalumane Chemical compound [Al+3].CCCC[O-].CCCC[O-].CCCC[O-] MYWQGROTKMBNKN-UHFFFAOYSA-N 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1275—Process of deposition of the inorganic material performed under inert atmosphere
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
Description
【発明の詳細な説明】 （イ）産業上の利用分野 本発明は窒化アルミニウム膜の形成方法に関する。[Detailed description of the invention] (b) Industrial application field The present invention relates to a method for forming an aluminum nitride film.
（ロ）従来の技術
窒化アルミニウム（ＡＪＮ）は高電気抵抗、高絶縁耐圧
、低誘電率、高熱伝導率、低熱膨張率などの％徴を持つ
素材で、放熱性の高い半導体用基板等に開発が進められ
ている。斯るＡＪＮ膜の形成方法は、Ｆ＠和６２年窒業
協会年会講演予稿集、３ＡＯ４、Ｐ、 ７０５〜７０６
に開示されている如く周知の減圧ＣＶＤ装置を用いてい
る。即ち、減圧した反応炉内に原料ガスのＡｊ？Ｃｊ？
５、ＮＨ５を導入し、これを熱分解することによって、
基板上にＡＪＮ膜を堆積するものである。(b) Conventional technology Aluminum nitride (AJN) is a material with characteristics such as high electrical resistance, high dielectric strength, low dielectric constant, high thermal conductivity, and low coefficient of thermal expansion, and has been developed as a substrate for semiconductors with high heat dissipation. is in progress. The method for forming such an AJN film is described in F@ Proceedings of the 1962 Annual Meeting of the Japan Nitrogen Industry Association, 3AO4, P, 705-706.
A well-known low pressure CVD apparatus is used as disclosed in . That is, the raw material gas Aj? Cj?
5. By introducing NH5 and thermally decomposing it,
An AJN film is deposited on a substrate.
ｅウ 発明が解決しようとする課題
しかし乍ら、斯る先行技術では反応炉内を減圧するため
の減圧手段が必要であるため、装置が大がかシなものに
なってしまい、製造コストが高くなる。さらにＡＩ！Ｎ
膜の形成前に反応炉内を一度高真空にするため、時間的
な損失が大きいという欠点を有している。eC Problems to be Solved by the Invention However, such prior art requires a pressure reduction means to reduce the pressure inside the reactor, which results in a large and bulky device, resulting in high manufacturing costs. It gets expensive. Even more AI! N
Since the inside of the reactor is once brought to a high vacuum before the film is formed, it has the disadvantage of a large time loss.
したがって、本発明は簡単な装置を用いることができ、
しかも形成時間の短いＡＪＮ膜の形成方法を提供するも
のである。Therefore, the present invention can use simple equipment,
Moreover, it provides a method for forming an AJN film that takes a short time to form.
に）課題を解決するための手段
本発明は、支持体上に窒化アルミニウム膜を形成する方
法であって、アルミニウムを含有した金属アルコキシド
を有機溶媒に溶かして溶液とし、該溶液に水を加えて上
記金属アルコキシドを加水分解させ、これを支持体に塗
布した後、窒素雰囲気中で熱処理することを特徴とする
。B) Means for Solving the Problems The present invention is a method for forming an aluminum nitride film on a support, the method comprising dissolving aluminum-containing metal alkoxide in an organic solvent to form a solution, and adding water to the solution. The method is characterized in that the metal alkoxide is hydrolyzed, applied to a support, and then heat-treated in a nitrogen atmosphere.
（ホ）作 用
上述の如く、本発明方法は気相反応を用いないため、反
応炉内を高真空にする必要はなくなる。(E) Function As mentioned above, since the method of the present invention does not use a gas phase reaction, there is no need to create a high vacuum in the reactor.
（へ）実施例
第１図に本発明形成方法に用いる加熱装置の一実施例を
示す。同図に於いて、（１）は石英等からなる耐熱性の
反応管、（２）及び（３）は夫々対向する反応管ｔｌｌ
の端部に配され、当該反応管（１）に窒素を導入、排気
するガス導入管及びガス排出管で、反応管（１）の端部
に栓体ｆ４１（４１で夫々接続されている。（５）は上
記反応管（１）の周囲に配さｎ１反応管は）内部を加熱
する電気ヒータ、（６）は所望のＡＪＮ膜を被着する支
持体、（７）は該支持体（６）を反応管はｊ内に載置す
るアルミナ等からなる載置台である。尚、斯る加熱装置
は何ら特別な構成を持つものではなく、後述するように
、１０００°Ｃ程度まで耐え得るものであればよい。(f) Example FIG. 1 shows an example of a heating device used in the forming method of the present invention. In the figure, (1) is a heat-resistant reaction tube made of quartz or the like, (2) and (3) are opposing reaction tubes, respectively.
A gas introduction pipe and a gas exhaust pipe are arranged at the end of the reaction tube (1) to introduce and exhaust nitrogen into the reaction tube (1), and are connected to the end of the reaction tube (1) by a stopper f41 (41). (5) is an electric heater arranged around the reaction tube (1) to heat the inside of the n1 reaction tube, (6) is a support on which the desired AJN film is coated, and (7) is the support ( 6) The reaction tube is a mounting table made of alumina or the like that is placed inside the tube. It should be noted that such a heating device does not have any special configuration, as long as it can withstand up to about 1000° C., as will be described later.
次に、本発明形成方法の一実施例を、化学反応式と共に
詳述する。Next, an example of the formation method of the present invention will be described in detail along with a chemical reaction formula.
先ず、ＡＪ（ＯＣ４Ｈ９）ｓ、ＡＪ（ＯＣ５Ｈ７）５←
、（ＣＨｊＯ）５ＡＪ等で表わされるアルミニウム含有
の金属アルコキシド、例えば人ｌ！（ＯＣ４Ｈ９） ５
を用意し、これにベンゼン等の有機溶剤を加えて溶かし
溶液状にする。そして、この溶液に水を加えて加水分解
させ、Ａｊ？（ＯＨ）３を生成する。この時の化学反応
は次式の通りである。First, AJ(OC4H9)s, AJ(OC5H7)5←
, (CHjO)5AJ, etc., such as aluminum! (OC4H9) 5
Prepare this and add an organic solvent such as benzene to it to dissolve it and make it into a solution. Then, water is added to this solution to cause hydrolysis, and Aj? (OH)3 is produced. The chemical reaction at this time is as shown in the following equation.
ＡＪ（ＯＣ４Ｈ９）３＋３Ｈｚ□→Ａ７（ＯＨ）３＋５
Ｃ４Ｈ９０１−ｆ次に、生成されたＡＩ！（ＯＨ〕ｓ溶
液にガラス等の支持体（６）を浸漬して支持体（６）表
面に溶液を塗布する。このように溶液中への支持体（６
）の浸漬を数回繰返すことによって、支持体（６）上に
塗布される溶液の量をある程度まで増やすことができ、
後に形成されるＡＪＮ膜の膜厚を１００μｍ程度まで変
えることができる。また、ＡＪ（０１−１）ａ溶液の塗
布法としては他に、スピンオン塗布法あるいはスプレー
法等を用いてもよい。AJ(OC4H9)3+3Hz□→A7(OH)3+5
C4H901-f Next, the generated AI! A support (6) such as glass is immersed in the (OH)s solution and the solution is applied to the surface of the support (6).In this way, the support (6) is dipped into the solution.
) By repeating dipping several times, the amount of solution applied onto the support (6) can be increased to a certain extent,
The thickness of the AJN film formed later can be varied up to about 100 μm. In addition, as a method for applying the AJ(01-1)a solution, a spin-on coating method, a spray method, or the like may be used.
次いで斯る支持体（６）を第１図に示した加熱装置内に
載置し、窒素雰囲気中で６００〜１０００°Ｃの加熱を
行う。これにより、支持体（６）表面に塗布されたｋｌ
ｃＯＨ）３とＮ２が反応し、支持体（６）表面に１０〜
１００μｍ程度の多結晶窒化アルミニウム（Ａ、ｇＮ）
膜が形成される。この時の化学反応は次式に示す通シで
ある。Next, the support (6) is placed in the heating device shown in FIG. 1, and heated at 600 to 1000°C in a nitrogen atmosphere. As a result, the kl applied to the surface of the support (6)
cOH)3 and N2 react, and 10~
Polycrystalline aluminum nitride (A, gN) about 100μm
A film is formed. The chemical reaction at this time is as shown in the following formula.
４−Ｖ（ＯＨ） ３＋２Ｎ２→４Ｍべ＋６Ｈ２０↑十幻
２↑通常ＡＩ！Ｎ膜は大方晶形の結晶構造であり、その
Ｃ軸が支持体（６）表面に垂直となれば、圧電特性を持
つようになる。即ち、斯るＡ７Ｎ膜表面に電極を設ける
ことによって弾性表面波素子として利用できる。ところ
で本発明者らが本発明形成方法において、加熱温度を変
えて種々実験を行ったところ、加熱温度の違いによって
支持体（６）表面に対するＡＡＮ膜結晶のＣ軸の方向が
変化することがわかった。そして、上述のようにＣ軸が
支持体（６）表面に垂直なＡＪＮ膜は加熱温度が１００
０°Ｃ＠後で得られた。4-V(OH) 3+2N2→4Mbe+6H20↑Jugen2↑Normal AI! The N film has an orthogonal crystal structure, and if its C axis is perpendicular to the surface of the support (6), it will have piezoelectric properties. That is, by providing electrodes on the surface of such A7N film, it can be used as a surface acoustic wave device. By the way, when the present inventors conducted various experiments by changing the heating temperature in the formation method of the present invention, it was found that the direction of the C axis of the AAN film crystal with respect to the surface of the support (6) changes depending on the difference in heating temperature. Ta. As mentioned above, the heating temperature of the AJN film whose C axis is perpendicular to the surface of the support (6) is 100.
Obtained after 0°C.
さらに、本発明形成方法はＡＪ（ＯＨ）ｘ溶液を支持体
（６）に塗布し、窒素雰囲気中で加熱するだけであるの
で、従来困難であった形状が複雑な支持体＋６） Ｋも
Ａｊ’（ＯＨ）ｓ溶液を容易に塗布することができ、所
望のＡＪＮ膜を形成することができる。Furthermore, since the forming method of the present invention only involves applying the AJ(OH) '(OH)s solution can be easily applied and a desired AJN film can be formed.
（ト）発明の効果
上述の説明から明らかな如く、本発明形成方法は、アル
ミニウム含有の金属アルコキシドを溶解及び加水分解し
、この溶液を支持体に塗布して窒素雰囲気中で加熱する
だけで容易ＫＡＪＮ膜が形成できる。即ち、本発明形成
方法で用いる装置は、窒素が導入できる、１０００°Ｃ
程度までの加熱装置であればよく、したがって装置が複
雑で犬がかシになることはない。また、反応管内を高真
空にすることもないので、全体のＡＪＮ膜形成時間も短
縮できる。(G) Effects of the Invention As is clear from the above explanation, the formation method of the present invention can be easily carried out by simply dissolving and hydrolyzing an aluminum-containing metal alkoxide, applying this solution to a support, and heating it in a nitrogen atmosphere. A KAJN film can be formed. That is, the apparatus used in the formation method of the present invention has a temperature of 1000°C where nitrogen can be introduced.
It is sufficient to use a heating device up to a certain level, so the device will not be complicated and cause the dog to become hungry. Furthermore, since the inside of the reaction tube is not required to be in a high vacuum, the overall AJN film formation time can also be shortened.
第１図は本発明形成方法に用いる加熱装置の一実施例を
示す断面図である。
ｔｌｌ・・・反応管、 （２）・・・ガス導入管、 １
３）・・・ガス排出管、 （４）・・・栓体、 （訃・
・電気ヒータ、 （６）・・・支持体、 （７）・・・
載置台。FIG. 1 is a sectional view showing an embodiment of a heating device used in the forming method of the present invention. tll...Reaction tube, (2)...Gas introduction tube, 1
3)...Gas exhaust pipe, (4)...Blug body, (Death/
・Electric heater, (6)...Support, (7)...
Mounting table.
Claims (1)
溶媒に溶かして溶液とし、該溶液に水を加えて上記金属
アルコキシドを加水分解させ、これを支持体に塗布した
後、窒素雰囲気中で熱処理することを特徴とする窒化ア
ルミニウム膜の形成方法。(1) A metal alkoxide containing aluminum is dissolved in an organic solvent to form a solution, water is added to the solution to hydrolyze the metal alkoxide, and this is applied to a support, followed by heat treatment in a nitrogen atmosphere. Characteristic method of forming aluminum nitride film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15174288A JPH01319682A (en) | 1988-06-20 | 1988-06-20 | Formation of aluminum nitride film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15174288A JPH01319682A (en) | 1988-06-20 | 1988-06-20 | Formation of aluminum nitride film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01319682A true JPH01319682A (en) | 1989-12-25 |
Family
ID=15525292
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15174288A Pending JPH01319682A (en) | 1988-06-20 | 1988-06-20 | Formation of aluminum nitride film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01319682A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994013853A1 (en) * | 1992-12-17 | 1994-06-23 | United Technologies Corporation | Metal nitride coated substrates |
| US5674304A (en) * | 1993-10-12 | 1997-10-07 | Semiconductor Energy Laboratory Co., Ltd. | Method of heat-treating a glass substrate |
-
1988
- 1988-06-20 JP JP15174288A patent/JPH01319682A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994013853A1 (en) * | 1992-12-17 | 1994-06-23 | United Technologies Corporation | Metal nitride coated substrates |
| US5674304A (en) * | 1993-10-12 | 1997-10-07 | Semiconductor Energy Laboratory Co., Ltd. | Method of heat-treating a glass substrate |
| US5929487A (en) * | 1993-10-12 | 1999-07-27 | Semiconductor Energy Laboratory Co., Ltd. | Glass substrate assembly, semiconductor device and method of heat-treating glass substrate |
| US6268631B1 (en) | 1993-10-12 | 2001-07-31 | Semiconductor Energy Laboratoty Co., Ltd. | Glass substrate assembly, semiconductor device and method of heat-treating glass substrate |
| US6847097B2 (en) | 1993-10-12 | 2005-01-25 | Semiconductor Energy Laboratory Co., Ltd. | Glass substrate assembly, semiconductor device and method of heat-treating glass substrate |
| US7038302B2 (en) | 1993-10-12 | 2006-05-02 | Semiconductor Energy Laboratory Co., Ltd. | Glass substrate assembly, semiconductor device and method of heat-treating glass substrate |
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