JPH0536440B2 - - Google Patents
Info
- Publication number
- JPH0536440B2 JPH0536440B2 JP16858787A JP16858787A JPH0536440B2 JP H0536440 B2 JPH0536440 B2 JP H0536440B2 JP 16858787 A JP16858787 A JP 16858787A JP 16858787 A JP16858787 A JP 16858787A JP H0536440 B2 JPH0536440 B2 JP H0536440B2
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- complex
- hexafluoropentanedionate
- forming
- alkaline earth
- 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 - Fee Related
Links
- 239000010409 thin film Substances 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 14
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 13
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 13
- 229910052788 barium Inorganic materials 0.000 claims description 7
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 229910052712 strontium Inorganic materials 0.000 claims description 6
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 239000000758 substrate Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000005234 chemical deposition Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 125000002524 organometallic group Chemical group 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 238000001947 vapour-phase growth Methods 0.000 description 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- PWHCIQQGOQTFAE-UHFFFAOYSA-L barium chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Ba+2] PWHCIQQGOQTFAE-UHFFFAOYSA-L 0.000 description 1
- 229910052454 barium strontium titanate Inorganic materials 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 238000005516 engineering process 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
- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Inorganic materials [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 1
- -1 strontium nitrate anhydride Chemical class 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Chemical Vapour Deposition (AREA)
Description
【発明の詳細な説明】
(産業上の利用分野)
本発明はアルカル土類金属の1,1,1,5,
5,5−ヘキサフルオロペンタンジオナート錯体
からなり、化学堆積法などで用いられる薄膜形成
用素材に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to alkaline earth metals such as 1, 1, 1, 5,
This invention relates to a material for forming thin films, which is made of a 5,5-hexafluoropentanedionate complex and is used in chemical deposition methods.
アルカル土類金属の1,1,1,5,5,5−
ヘキサフルオロペンタンジオナート錯体の報告は
まだかつてされた例がない。
1,1,1,5,5,5- of alkaline earth metals
There have been no reports of hexafluoropentanedionate complexes yet.
本発明者は、鋭意研究を行つた結果、アルカリ
土類金属の1,1,1,5,5,5−ヘキサフル
オロペンタンジオナート錯体が薄膜形成用素材と
して有用であることを見い出し本発明を完成し
た。 As a result of extensive research, the present inventor discovered that an alkaline earth metal 1,1,1,5,5,5-hexafluoropentanedionate complex is useful as a material for forming a thin film, and has developed the present invention. completed.
すなわち、本発明の要旨は紫外線吸収測定装置
により測定された吸収波長が240nm〜350nmで
あるアルカリ土類金属の1,1,1,5,5,5
−ヘキサフルオロペンタンジオナート錯体からな
る薄膜形成用素材に存する。
That is, the gist of the present invention is to obtain 1,1,1,5,5,5 alkaline earth metals having an absorption wavelength of 240 nm to 350 nm as measured by an ultraviolet absorption measuring device.
- A material for forming a thin film comprising a hexafluoropentanedionate complex.
以下本発明について更に詳しく説明する。 The present invention will be explained in more detail below.
本発明に係る薄膜形成用素材は、アルカリ土類
金属の1,1,1,5,5,5−ヘキサフルオロ
ペンタンジオナート錯体からなるもので、これに
より気相化学堆積法のような錯体の蒸気を利用し
た薄膜形成を可能ならしめたものである。 The material for forming a thin film according to the present invention is composed of a 1,1,1,5,5,5-hexafluoropentanedionate complex of an alkaline earth metal. This makes it possible to form thin films using steam.
ここで、アルカリ土類金属の1,1,1,5,
5,5−ヘキサフルオロペンタンジオナート錯体
としては1,1,1,5,5,5−ヘキサフルオ
ロ−2,4−ペンタンジオナートバリウム錯体又
は1,1,1,5,5,5−ヘキサフルオロ−
2,4−ペンタンジオナートストロンチウム錯体
がある。 Here, 1, 1, 1, 5,
The 5,5-hexafluoropentanedionate complex includes 1,1,1,5,5,5-hexafluoro-2,4-pentanedionate barium complex or 1,1,1,5,5,5-hexafluoro-2,4-pentanedionate barium complex. Fluoro-
There is a 2,4-pentanedionate strontium complex.
また、アルカリ土類金属の1,1,1,5,
5,5−ヘキサフルオロペンタンジオナート錯体
としては紫外線吸収測定装置で測定した吸収波長
が240nm〜350nmである。 In addition, alkaline earth metals 1, 1, 1, 5,
The 5,5-hexafluoropentanedionate complex has an absorption wavelength of 240 nm to 350 nm as measured by an ultraviolet absorption measuring device.
更に、アルカリ土類金属の1,1,1,5,
5,5−ヘキサフルオロペンタンジオナート錯体
としては蒸気圧が100℃で40〜200mmHg、好まし
くは80〜160mmHgのものを用いることが好まし
い。 Furthermore, alkaline earth metals 1, 1, 1, 5,
As the 5,5-hexafluoropentanedionate complex, it is preferable to use one having a vapor pressure of 40 to 200 mmHg, preferably 80 to 160 mmHg at 100°C.
また、アルカリ土類金属の1,1,1,5,
5,5−ヘキサフルオロペンタンジオナート錯体
は、不純物を少なくするため昇華精製したものを
用いることが好ましい。 In addition, alkaline earth metals 1, 1, 1, 5,
It is preferable to use a 5,5-hexafluoropentanedionate complex that has been purified by sublimation in order to reduce impurities.
本発明のアルカリ土類金属の1,1,1,5,
5,5−ヘキサフルオロペンタンジオナート錯体
の製造に関する報告はない。 1, 1, 1, 5, of the alkaline earth metal of the present invention
There are no reports regarding the production of 5,5-hexafluoropentanedionate complexes.
本発明の薄膜形成用素材を使用して薄膜を形成
する場合、液相堆積法または気相堆積法がある
が、特に気相堆積法が好ましい。 When forming a thin film using the thin film forming material of the present invention, a liquid phase deposition method or a vapor phase deposition method may be used, and the vapor phase deposition method is particularly preferred.
本発明の薄膜形成用素材を使用して薄膜を形成
する場合、加圧下または常圧下または減圧下のい
ずれも可能であるが、常圧下または減圧下が好ま
しい。 When forming a thin film using the material for forming a thin film of the present invention, it is possible to form a thin film under pressure, normal pressure, or reduced pressure, but normal pressure or reduced pressure is preferable.
本発明の薄膜形成用素材を使用して薄膜を形成
する場合、基板はアルミナ、窒化アルミニウム、
酸化ケイ素、酸化マグネシウム、酸化ジルコニウ
ム、チタン酸バリウム、チタン酸ストロンチウム
などがある。 When forming a thin film using the thin film forming material of the present invention, the substrate may be alumina, aluminum nitride,
These include silicon oxide, magnesium oxide, zirconium oxide, barium titanate, and strontium titanate.
本発明の薄膜形成用素材を使用して薄膜を形成
する場合、基板の温度は400℃〜1000℃であるが、
600℃〜800℃が好ましい。 When forming a thin film using the thin film forming material of the present invention, the temperature of the substrate is 400°C to 1000°C;
600°C to 800°C is preferred.
本発明の薄膜形成用素材を使用して薄膜を形成
する場合、照射する紫外線の波長は190nm〜
350nmである。 When forming a thin film using the thin film forming material of the present invention, the wavelength of the irradiated ultraviolet rays is 190 nm ~
It is 350nm.
本発明の薄膜形成用素材を使用して薄膜を形成
する場合、同伴ガスは酸素、空気、ヘリウム、ア
ルゴン、窒素の1種または2種以上の混合ガスで
ある。 When forming a thin film using the material for forming a thin film of the present invention, the accompanying gas is one or a mixture of two or more of oxygen, air, helium, argon, and nitrogen.
次にアルカリ土類金属の1,1,1,5,5,
5−ヘキサフルオロペンタンジオナート錯体の製
造の一例を示す。
Next, alkaline earth metals 1, 1, 1, 5, 5,
An example of the production of a 5-hexafluoropentanedionate complex is shown.
製造例 1
1,1,1,5,5,5−ヘキサフルオロペン
タンジオナートバリウム錯体の製造
5.8gの塩化バリウム・2水物を溶解させた水
溶液15mlを室温で攪拌し、これに1,1,1,
5,5,5−ヘキサフルオロ−2,4−ペンタン
ジオンを10.0g加えて、12時間攪拌することによ
り、無色透明又は白色の固体が生成した。この無
色透明又は白色の固体を過し、さらにヘキサン
10mlで洗浄した。Production Example 1 Production of 1,1,1,5,5,5-hexafluoropentanedionate barium complex 15 ml of an aqueous solution in which 5.8 g of barium chloride dihydrate was dissolved was stirred at room temperature, and 1,1 ,1,
A colorless transparent or white solid was produced by adding 10.0 g of 5,5,5-hexafluoro-2,4-pentanedione and stirring for 12 hours. This colorless transparent or white solid is filtered and then hexane is added.
Washed with 10ml.
さらに、90〜100℃で、130mmHgという減圧条
件下で昇華させることにより、本発明の1,1,
1,5,5,5−ヘキサフルオロペンタンジオナ
ートバリウム錯体を得た。 Furthermore, by sublimating at 90 to 100°C and under reduced pressure conditions of 130 mmHg,
A 1,5,5,5-hexafluoropentanedionate barium complex was obtained.
製造例 2
1,1,1,5,5,5−ヘキサフルオロペン
タンジオナートストロンチウム錯体の製造
5.0gの硝酸ストロンチウム・無水物を溶解さ
せた水溶液20mlを室温で攪拌し、これに1,1,
1,5,5,5−ヘキサフルオロ−2,4−ペン
タンジオンを10g加えて12時間攪拌することによ
り、無色透明又は白色の固体が生成した。この無
色透明又は白色の固体を過し、さらにヘキサン
10mlで洗浄した。Production Example 2 Production of 1,1,1,5,5,5-hexafluoropentanedionate strontium complex 20 ml of an aqueous solution in which 5.0 g of strontium nitrate anhydride was dissolved was stirred at room temperature, and 1,1,
A colorless transparent or white solid was produced by adding 10 g of 1,5,5,5-hexafluoro-2,4-pentanedione and stirring for 12 hours. This colorless transparent or white solid is filtered and then hexane is added.
Washed with 10ml.
さらに90〜100℃で、100mmHgという減圧条件
下で昇華させることにより、本発明の1,1,
1,5,5,5−ヘキサフルオロペンタンジオナ
ートストロンチウム錯体を得た。 Further, by sublimating at a temperature of 90 to 100°C and a reduced pressure of 100 mmHg, 1, 1,
A 1,5,5,5-hexafluoropentanedionate strontium complex was obtained.
薄膜の組成分析は、X線光電子分光装置
(XPS)を用いて行つた。 The compositional analysis of the thin film was performed using an X-ray photoelectron spectrometer (XPS).
薄膜の膜厚測定は電子顕微鏡を用いた。 An electron microscope was used to measure the thickness of the thin film.
次に実施例を示し、本発明の効果を具体的に説
明する。 Next, examples will be shown to specifically explain the effects of the present invention.
実施例 1
有機金属気相化学堆積法用の装置を用い、酸化
ケイ素の基板を高周波誘導加熱装置で800℃に熱
した後、1,1,1,5,5,5−ヘキサフルオ
ロペンタンジオナートバリウム錯体の入つた容器
を50℃に保ちながら酸素を20ml/minの一定速度
で流し容器より出たガスを基板のある反応室へ送
つた。基板上で1,1,1,5,5,5−ヘキサ
フルオロペンタンジオナートバリウム錯体が分解
し、酸化バリウムの薄膜が形成された。この膜厚
を測定すると2μmであつた。Example 1 Using an apparatus for organometallic vapor phase chemical deposition, a silicon oxide substrate was heated to 800°C with a high frequency induction heating apparatus, and then 1,1,1,5,5,5-hexafluoropentanedionate was heated. While maintaining the container containing the barium complex at 50°C, oxygen was flowed at a constant rate of 20 ml/min, and the gas released from the container was sent to the reaction chamber where the substrate was located. The 1,1,1,5,5,5-hexafluoropentanedionate barium complex was decomposed on the substrate to form a thin film of barium oxide. The thickness of this film was measured to be 2 μm.
実施例 2
有機金属気相化学堆積法の装置を用い酸化アル
ミニウムの基板を200℃に熱した後、重水素ラン
プを基板に照射しながら1,1,1,5,5,5
−ヘキサフルオロペンタンジオナートストロンチ
ウム錯体の入つた容器を50℃に保ちながら酸素を
20ml/minの一定速度で流し、容器より出たガス
を基板のある反応室へ送つた。基板上で1,1,
1,5,5,5−ヘキサフルオロペンタンジオナ
ートストロンチウム錯体が分解し、酸化ストロン
チウムの薄膜が形成された。この膜厚を測定する
と1μmであつた。Example 2 After heating an aluminum oxide substrate to 200°C using an organometallic vapor phase chemical deposition apparatus, 1, 1, 1, 5, 5, 5 was applied while irradiating the substrate with a deuterium lamp.
- Oxygen is added to the container containing the hexafluoropentanedionate strontium complex while keeping it at 50℃.
The gas was flowed at a constant rate of 20 ml/min, and the gas coming out of the container was sent to the reaction chamber where the substrate was located. 1, 1, on the board
The 1,5,5,5-hexafluoropentanedionate strontium complex decomposed and a thin film of strontium oxide was formed. The thickness of this film was measured to be 1 μm.
Claims (1)
長が240nm〜350nmであるアルカリ土類金属の
1,1,1,5,5,5−ヘキサフルオロペンタ
ンジオナート錯体からなる薄膜形成用素材。 2 該アルカリ土類金属がバリウムである特許請
求第1項記載の薄膜形成用素材。 3 該アルカリ土類金属がストロンチウムである
特許請求第1項記載の薄膜形成用素材。 4 該錯体の蒸気圧が100℃で40〜200mmHgであ
る特許請求第1項記載の薄膜形成用素材。[Scope of Claims] 1. Formation of a thin film made of a 1,1,1,5,5,5-hexafluoropentanedionate complex of an alkaline earth metal whose absorption wavelength is 240 nm to 350 nm as measured by an ultraviolet absorption measuring device. Material for use. 2. The material for forming a thin film according to claim 1, wherein the alkaline earth metal is barium. 3. The material for forming a thin film according to claim 1, wherein the alkaline earth metal is strontium. 4. The material for forming a thin film according to claim 1, wherein the complex has a vapor pressure of 40 to 200 mmHg at 100°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16858787A JPS6416742A (en) | 1987-07-08 | 1987-07-08 | Thin film-forming material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16858787A JPS6416742A (en) | 1987-07-08 | 1987-07-08 | Thin film-forming material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6416742A JPS6416742A (en) | 1989-01-20 |
| JPH0536440B2 true JPH0536440B2 (en) | 1993-05-31 |
Family
ID=15870822
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16858787A Granted JPS6416742A (en) | 1987-07-08 | 1987-07-08 | Thin film-forming material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6416742A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2551860B2 (en) * | 1990-09-25 | 1996-11-06 | 東ソー・アクゾ株式会社 | Metal complex for thin film formation |
-
1987
- 1987-07-08 JP JP16858787A patent/JPS6416742A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6416742A (en) | 1989-01-20 |
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