JPH0455129B2 - - Google Patents
Info
- Publication number
- JPH0455129B2 JPH0455129B2 JP7121286A JP7121286A JPH0455129B2 JP H0455129 B2 JPH0455129 B2 JP H0455129B2 JP 7121286 A JP7121286 A JP 7121286A JP 7121286 A JP7121286 A JP 7121286A JP H0455129 B2 JPH0455129 B2 JP H0455129B2
- Authority
- JP
- Japan
- Prior art keywords
- alumina
- spray
- thin film
- film
- alumina thin
- 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.)
- Expired
Links
- 239000007921 spray Substances 0.000 claims description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 21
- 239000010409 thin film Substances 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 239000010408 film Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000007733 ion plating Methods 0.000 description 2
- -1 monoethyl acetoacetate aluminum diacetate Chemical compound 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
Landscapes
- Application Of Or Painting With Fluid Materials (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、例えば遠赤外線放射膜、熱線反射
膜、絶縁性膜等として用いられるアルミナ薄膜の
製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing an alumina thin film used as, for example, a far-infrared emitting film, a heat ray reflecting film, an insulating film, and the like.
（従来の技術）
従来、この種のアルミナ薄膜の製造方法として
は、酸化アルミニウムのスパツタリング法やイオ
ンプレーテイング法等のPVD法、或いは有機金
属化合物のデイツプ法等が知られている。(Prior Art) Conventionally, known methods for producing this type of alumina thin film include PVD methods such as aluminum oxide sputtering and ion plating methods, and organometallic compound dip methods.
（発明が解決しようとする問題点）
前記従来のスパツタリング法やイオンプレーテ
イング法の場合、装置的に大がかりとなり、更に
真空槽で行なうため、製造されるアルミナ薄膜の
大きさが制限されると共に非常にコストアツプと
なる不都合を有し、またデイツプ法の場合、引上
げ操作が難しく膜質が悪く、また密着性にも欠け
るという不都合を有する。(Problems to be Solved by the Invention) In the case of the conventional sputtering method and ion plating method, the equipment is large-scale and the process is carried out in a vacuum chamber, which limits the size of the alumina thin film produced and makes it very difficult to produce. In addition, in the case of the dip method, the pulling operation is difficult, the film quality is poor, and adhesion is also lacking.
（問題点を解決するための手段）
本発明は、前記不都合を解消したアルミナ薄膜
の製造方法を提供することを目的とするもので、
その発明は、一般式（AcO）ｘ（RO）２−xAl
（R′COCHCOOR″）（ただし、式中ｘは１または
２であり、ＲはC2H5、C3H7、C4H9を示し、R′、
R″はCH3、C2H5、C3H7、C4H9、C6H5、C8H17
を示す）で表わされるアルコキシアセテートアル
ミニウムβ−ケトエステルを有機溶媒中に含むス
プレー溶液を400〜700℃に保たれた基材上に噴霧
してアルミナ薄膜を形成することから成る。(Means for Solving the Problems) An object of the present invention is to provide a method for manufacturing an alumina thin film that eliminates the above-mentioned disadvantages.
The invention is based on the general formula (AcO)x(RO)2−xAl
(R′COCHCOOR″) (in the formula, x is 1 or 2, R represents C 2 H 5 , C 3 H 7 , C 4 H 9 , R′,
R″ is CH 3 , C 2 H 5 , C 3 H 7 , C 4 H 9 , C 6 H 5 , C 8 H 17
The process consists of spraying a spray solution containing an alkoxyacetate aluminum β-ketoester represented by the following formula in an organic solvent onto a substrate kept at 400 to 700°C to form an alumina thin film.
前記アルコキシアセテートアルミニウムβ−ケ
トエステルの一般式中、ｘは１または２としたの
は、ｘが０では熱分解しにくくなり、またｘが３
以上となると有機溶媒への溶解度が悪くなるから
である。尚、ｘが１の方が有機溶媒への溶解性に
優れ、またｘが２の方がより酸化物になりやす
い。 In the general formula of the alkoxyacetate aluminum β-ketoester, x is set to 1 or 2 because if x is 0, it will be difficult to thermally decompose, and if x is 3
This is because the solubility in organic solvents deteriorates when the amount exceeds the range. Note that when x is 1, the solubility in organic solvents is better, and when x is 2, it is easier to form an oxide.
スプレー溶液は、前記アルコキシアセテートア
ルミニウムβ−ケトエステルが有機溶媒、好まし
くはベンゼン溶媒中にアルミナ（Al2O3）含有量
換算で１〜10wt％、好ましくは２〜5wt％程度と
なるように調整する。アルミナ（Al2O3）含有量
が1wt％未満であると成膜効率が悪く、また10wt
％を越えるとスプレー溶液の粘度が高くなり作業
性が悪くなるからである。 The spray solution is adjusted so that the alkoxyacetate aluminum β-ketoester is in an organic solvent, preferably a benzene solvent, so that the alumina (Al 2 O 3 ) content is about 1 to 10 wt%, preferably about 2 to 5 wt%. . If the alumina (Al 2 O 3 ) content is less than 1wt%, the film formation efficiency will be poor;
%, the viscosity of the spray solution increases and workability deteriorates.
基材は、特に限定されるものではないが、一般
にはガラス、セラミツク等の板状体を用い、これ
を400〜700℃、好ましくは400〜600゜に加熱して
おいてから前記スプレー溶液を噴霧する。基材が
400℃未満であると膜は粉体のまじつたものにな
り易く、また700℃を越えると膜化せずに粉体と
なり易いからである。また、予め400〜700℃に加
熱された基材上にスプレー溶液を噴霧するので、
基材上に付着するスプレー溶液は付着と同時に順
次熱分解され、CVD法と同様に、熱力学的平衡
状態で成膜が進行し、均一で透明なアルミナ薄膜
が形成される。 The base material is not particularly limited, but generally a plate-like material such as glass or ceramic is used, which is heated to 400 to 700°C, preferably 400 to 600°, and then the spray solution is applied. Spray. The base material
This is because if the temperature is less than 400°C, the film tends to become a mixture of powder, and if it exceeds 700°C, it tends to become powder without forming a film. In addition, since the spray solution is sprayed onto the substrate that has been preheated to 400-700℃,
The spray solution that adheres to the substrate is sequentially thermally decomposed at the same time as it adheres, and like the CVD method, film formation proceeds in a thermodynamic equilibrium state, forming a uniform and transparent alumina thin film.
スプレー溶液は、一般にはスプレー圧を0.5〜
1.5Kg／cm2で噴霧する。 Spray solutions generally have a spray pressure of 0.5~
Spray at 1.5Kg/ cm2 .
（実施例） 次に、本発明の実施例に付き説明する。(Example) Next, examples of the present invention will be explained.
実施例 １
アルミナ（Al2O3）含有量換算で2.5wt％モノ
エチルアセトアセテートアルミニウジアセテート
をベンゼン溶媒中に含ませたスプレー溶液を用意
し、スプレー圧1.0Kg／cm2、スプレー距離50cmで、
450℃に加熱された板状のセラミツク基材上に
種々の吹付量で噴霧して、種々の膜厚のアルミナ
薄膜を得た。得られたアルミナ薄膜は、全て、透
明で傷付きにくく、密着性にも優れ、しかもピン
ホール等の全くない均一な薄膜であつた。Example 1 A spray solution containing 2.5wt% monoethyl acetoacetate aluminum diacetate in terms of alumina (Al 2 O 3 ) content in a benzene solvent was prepared and sprayed at a spray pressure of 1.0 Kg/cm 2 and a spray distance of 50 cm. ,
Alumina thin films of various thicknesses were obtained by spraying at various spray rates onto a plate-shaped ceramic substrate heated to 450°C. All of the obtained alumina thin films were transparent, hard to scratch, had excellent adhesion, and were uniform thin films with no pinholes or the like.
図面はスプレー溶液の吹付量と膜厚の関係を示
すグラフであり、吹付量と膜厚はほぼ正比例して
おり、膜厚の制御が容易に行なえることがわか
る。 The figure is a graph showing the relationship between the amount of spray solution and the film thickness, and it can be seen that the amount of sprayed solution and the film thickness are almost directly proportional, and that the film thickness can be easily controlled.
実施例 ２
アルミナ（Al2O3）含有量換算で10wt％のイソ
プロポキシアセテートアルミニウムエチルアセト
アセテートをイソプロパノール溶媒中に含ませた
スプレー溶液を用意し、スプレー圧1.0Kg／cm2、
スプレー距離50cmで、550℃に加熱された板状の
セラミツク基材上に種々の吹付量で噴霧して、
種々の膜厚のアルミナ薄膜を得た。得られたアル
ミナ薄膜は、全て、透明で傷付きにくく、密着性
にも優れ、しかもピンホール等が全くない均一な
薄膜であつた。Example 2 A spray solution containing 10 wt% isopropoxy acetate aluminum ethyl acetoacetate in terms of alumina (Al 2 O 3 ) content in isopropanol solvent was prepared, and the spraying pressure was 1.0 Kg/cm 2 .
At a spray distance of 50cm, spray at various amounts onto a plate-shaped ceramic substrate heated to 550℃.
Alumina thin films of various thicknesses were obtained. All of the obtained alumina thin films were transparent, hard to scratch, had excellent adhesion, and were uniform thin films with no pinholes or the like.
（発明の効果）
このように、本発明によれば前記特定のアルコ
キシアセテートアルミニウムβ−ケトエステルを
有機溶媒中に含むスプレー溶液を400〜700℃に保
たれた基材上に噴霧してアルミナ薄膜を形成する
ようにしたので、極めて簡単な方法で、厚みの小
さなアルミナ薄膜を、CVD法並みの均一さと密
着性とをもつて、しかも大面積のものも製造でき
る効果を有する。(Effects of the Invention) According to the present invention, a thin alumina film is formed by spraying a spray solution containing the specific alkoxyacetate aluminum β-ketoester in an organic solvent onto a substrate kept at 400 to 700°C. This method has the effect of producing a small alumina thin film with uniformity and adhesion comparable to that of the CVD method, and also over a large area, using an extremely simple method.
図面は本発明製造方法の１実施例によつて得ら
れたアルミナ薄膜のスプレー吹付量と膜厚との関
係を示すグラフである。
The drawing is a graph showing the relationship between the spray amount and film thickness of an alumina thin film obtained by one embodiment of the manufacturing method of the present invention.
Claims (1)
（R′COCHCOOR″）（ただし、式中ｘは１または
２であり、ＲはC2H5、C3H7、C4H9を示し、R′、
R″はCH3、C2H5、C3H7、C4H9、C6H5、C8H17
を示す）で表わされるアルコキシアセテートアル
ミニウムβ−ケトエステルを有機溶媒中に含むス
プレー溶液を400〜700℃に保たれた基材上に噴霧
してアルミナ薄膜を形成することから成るアルミ
ナ薄膜の製造方法。 ２ 該アルコキシアセテートアルミニウムβ−ケ
トエステルをアルミナ（Al2O3）含有量換算で１
〜10wt％含むスプレー溶液を用いることを特徴
とする特許請求の範囲第１項に記載のアルミナ薄
膜の製造方法。[Claims] 1 General formula (AcO)x(RO)2-xAl
(R′COCHCOOR″) (in the formula, x is 1 or 2, R represents C 2 H 5 , C 3 H 7 , C 4 H 9 , R′,
R″ is CH 3 , C 2 H 5 , C 3 H 7 , C 4 H 9 , C 6 H 5 , C 8 H 17
1. A method for producing an alumina thin film, which comprises spraying a spray solution containing an alkoxyacetate aluminum β-ketoester represented by the following formula in an organic solvent onto a substrate kept at 400 to 700°C to form an alumina thin film. 2 The alkoxyacetate aluminum β-ketoester is 1 in terms of alumina (Al 2 O 3 ) content.
The method for producing an alumina thin film according to claim 1, characterized in that a spray solution containing ~10 wt% is used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7121286A JPS62227478A (en) | 1986-03-31 | 1986-03-31 | Production of alumina membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7121286A JPS62227478A (en) | 1986-03-31 | 1986-03-31 | Production of alumina membrane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62227478A JPS62227478A (en) | 1987-10-06 |
| JPH0455129B2 true JPH0455129B2 (en) | 1992-09-02 |
Family
ID=13454148
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7121286A Granted JPS62227478A (en) | 1986-03-31 | 1986-03-31 | Production of alumina membrane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62227478A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4797356B2 (en) * | 2004-09-30 | 2011-10-19 | 日油株式会社 | Aluminum oxide thin film and composition for forming aluminum oxide thin film |
-
1986
- 1986-03-31 JP JP7121286A patent/JPS62227478A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62227478A (en) | 1987-10-06 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |