JPH0517874A - Formation of superfine particle dispersed film under grain size control - Google Patents
Formation of superfine particle dispersed film under grain size controlInfo
- Publication number
- JPH0517874A JPH0517874A JP16985391A JP16985391A JPH0517874A JP H0517874 A JPH0517874 A JP H0517874A JP 16985391 A JP16985391 A JP 16985391A JP 16985391 A JP16985391 A JP 16985391A JP H0517874 A JPH0517874 A JP H0517874A
- Authority
- JP
- Japan
- Prior art keywords
- film thickness
- film
- particle size
- substrate
- raw material
- 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.)
- Withdrawn
Links
- 239000002245 particle Substances 0.000 title claims abstract description 36
- 230000015572 biosynthetic process Effects 0.000 title claims description 3
- 239000010408 film Substances 0.000 claims abstract description 68
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 238000001704 evaporation Methods 0.000 claims abstract description 17
- 239000010409 thin film Substances 0.000 claims abstract description 15
- 230000008020 evaporation Effects 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000011882 ultra-fine particle Substances 0.000 claims description 24
- 239000000523 sample Substances 0.000 claims description 2
- 238000000151 deposition Methods 0.000 abstract description 2
- 239000010931 gold Substances 0.000 description 16
- 229910004298 SiO 2 Inorganic materials 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、非線形光学材料の超微
粒子分散膜の粒径制御成膜方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for controlling the particle size of ultrafine particle dispersion films of nonlinear optical materials.
【０００２】[0002]
【従来の技術】従来の成膜方法においては、装置条件に
より超微粒子の粒径を制御しており、製造中に粒径をモ
ニターする方法はなかった。また、膜厚計の表示膜厚を
薄膜形成初期における粒径の制御モニターとして使用す
る例はなかった。2. Description of the Related Art In the conventional film forming method, the particle size of ultrafine particles is controlled by the apparatus conditions, and there is no method for monitoring the particle size during manufacturing. Moreover, there is no example in which the displayed film thickness of the film thickness meter is used as a monitor for controlling the particle size in the initial stage of thin film formation.
【０００３】[0003]
【発明が解決しようとする課題】従来の超微粒子分散膜
の成膜方法においては、粒径をモニターする手法がない
ため、粒径を制御し再現性よく製造しようとするには、
装置条件をすべて同一にする必要があるが、装置条件を
同一にしても微妙な運転条件の違いがあるため、再現性
よく超微粒子分散膜を製造することができなかった。In the conventional method for forming an ultrafine particle dispersion film, there is no method for monitoring the particle size. Therefore, in order to control the particle size and manufacture with good reproducibility,
It is necessary to make all the apparatus conditions the same, but even if the apparatus conditions are made the same, there are subtle differences in the operating conditions, so that it was not possible to manufacture the ultrafine particle dispersed film with good reproducibility.
【０００４】本発明は上記の課題を解決しようとするも
のである。The present invention is intended to solve the above problems.
【０００５】[0005]
【課題を解決するための手段】本発明の超微粒子分散膜
の粒径制御成膜方法は、基板と蒸発源が内部に設けられ
た真空容器中の上記基板の近傍に膜厚計の測定子を配設
し、予め膜厚計の表示膜厚と基板表面に蒸着される薄膜
原料の粒径との関係をもとめた後、基板に形成される分
散膜の膜厚を上記膜厚計により測定しながら蒸発源から
薄膜原料を蒸発させ、上記予め求めた膜厚計の表示膜厚
と薄膜原料の粒径との関係より所定の粒径に対応した表
示膜厚となるまで薄膜原料を基板に蒸着させることを特
徴としている。According to the present invention, there is provided a method for controlling the particle size of an ultrafine particle dispersed film, wherein a film thickness gauge probe is provided in the vicinity of the substrate in a vacuum container in which the substrate and an evaporation source are provided. After determining the relationship between the displayed film thickness of the film thickness meter and the particle size of the thin film raw material deposited on the substrate surface in advance, measure the film thickness of the dispersion film formed on the substrate with the above film thickness meter. While evaporating the thin film raw material from the evaporation source, the thin film raw material is applied to the substrate until the display film thickness corresponding to the predetermined particle diameter is obtained from the relationship between the previously determined display film thickness of the film thickness gauge and the particle diameter of the thin film raw material. It is characterized by vapor deposition.
【０００６】[0006]
【作用】上記において、蒸発源より蒸発し基板面に生成
される超微粒子の粒径は、基板に蒸着する薄膜原料の量
が多くなるほど大きくなるため、超微粒子の粒径と膜厚
計の表示膜厚との間には対応関係がある。そのため、膜
厚計が所定の表示膜厚を示すまで、蒸発源から蒸発した
薄膜原料を基板面に蒸着させ分散膜を形成させることに
より、所定の粒径の超微粒子からなる分散膜とすること
ができる。In the above, the particle size of the ultrafine particles evaporated from the evaporation source and generated on the substrate surface becomes larger as the amount of the thin film raw material deposited on the substrate becomes larger. There is a correspondence relationship with the film thickness. Therefore, a thin film raw material evaporated from an evaporation source is vapor-deposited on the substrate surface to form a dispersed film until the film thickness meter shows a predetermined display film thickness, thereby forming a dispersed film composed of ultrafine particles of a predetermined particle size. You can
【０００７】上記により、超微粒子の粒径をコントロー
ルすることができ、再現性のよい超微粒子分散膜の成膜
方法を実現する。As described above, the particle size of the ultrafine particles can be controlled, and a method for forming an ultrafine particle dispersed film with good reproducibility is realized.
【０００８】[0008]
【実施例】本発明の一実施例に適用される装置につい
て、図１により説明する。図１において、１は真空容器
であり、３は同真空容器１内下部に設けられ金Ａｕ及び
二酸化ケイ素ＳｉＯ2 を蒸発する蒸発源、２は上記真空
容器１内上部に設けられ蒸発源３より蒸発したＡｕおよ
びＳｉＯ2 を捕集するＳｉＯ2 基板、４は上記真空容器
１内側部に設けられた水晶振動子膜厚計の膜厚測定子で
ある。DESCRIPTION OF THE PREFERRED EMBODIMENTS An apparatus applied to one embodiment of the present invention will be described with reference to FIG. In FIG. 1, 1 is a vacuum container, 3 is an evaporation source provided in the lower part of the vacuum container 1 for evaporating gold Au and silicon dioxide SiO 2 , and 2 is an evaporation source provided in the upper part of the vacuum container 1 from the evaporation source 3. The SiO 2 substrates 4 that collect the evaporated Au and SiO 2 are film thickness gauges of a quartz oscillator film thickness meter provided inside the vacuum container 1.
【０００９】上記において、蒸発源３より蒸発しＳｉＯ
2 基板２面に生成されるＡｕ超微粒子の粒径はＳｉＯ2
基板２に蒸着するＡｕの量が多くなるほど大きくなるた
め、Ａｕ超微粒子の粒径と膜厚計により表示される膜厚
との間には対応関係がある。この関係を実験により求め
たものが、図２に示すグラフである。In the above, SiO is evaporated from the evaporation source 3.
2 The particle size of the ultrafine Au particles generated on the 2nd surface of the substrate is SiO 2
Since the larger the amount of Au deposited on the substrate 2 is, the larger the amount of Au deposited, and therefore, there is a correspondence relationship between the particle size of the Au ultrafine particles and the film thickness displayed by the film thickness meter. The relationship shown in FIG. 2 is obtained by experiment.
【００１０】本実施例においては、予め図２に示すＡｕ
超微粒子の粒径と膜厚計の表示膜厚の関係を求めてお
き、膜厚計の表示膜厚が５Åとなるまで蒸発源３よりＡ
ｕを蒸発させ、ＳｉＯ2 基板２面に粒径が３０ÅのＡｕ
超微粒子を生成した膜を形成させた。続いて、蒸発源３
よりＳｉＯ2 を蒸発させて上記Ａｕ超微粒子の上に蒸着
させ、同Ａｕ超微粒子を十分覆う程度の膜厚（５００
Å）まで成膜させた。In this embodiment, the Au shown in FIG.
The relationship between the particle size of the ultra-fine particles and the display film thickness of the film thickness meter is obtained in advance.
u is evaporated, and Au with a particle size of 30Å is deposited on the SiO 2 substrate 2 surface.
A film having ultrafine particles was formed. Then, evaporation source 3
SiO 2 is evaporated and vapor-deposited on the Au ultrafine particles to obtain a film thickness (500 μm) sufficient to cover the Au ultrafine particles.
Films were formed up to Å).
【００１１】上記により得られた薄膜は、粒径３０Åの
Ａｕ超微粒子がＳｉＯ2 中に分散した薄膜であり、本実
施例と同一方法で数回くり返し成膜を行なったところ、
いずれの場合も上記と同様の分散膜を得ることができ、
再現性があることが判った。The thin film obtained as described above is a thin film in which ultrafine Au particles having a particle size of 30 Å are dispersed in SiO 2. The film was repeatedly formed several times by the same method as in this example.
In any case, a dispersion film similar to the above can be obtained,
It turned out to be reproducible.
【００１２】また、上記と同様の方法で、Ａｕ超微粒子
の粒径が２０Å，４０Å，５０Åになるような膜厚計の
表示膜厚で成膜を行い、それぞれ２０Å，４０Å，５０
ÅのＡｕ超微粒子分散膜を成膜することができた。In the same manner as described above, the Au ultrafine particles are formed into a film thickness of 20 Å, 40 Å and 50 Å, and the film thickness is indicated by 20 Å, 40 Å and 50 Å, respectively.
The Au ultrafine particle dispersion film of Å could be formed.
【００１３】上記により、Ａｕ超微粒子の粒径をコント
ロールすることができ、再現性のよいＡｕ超微粒子分散
膜の成膜方法を実現した。As described above, the particle size of the Au ultrafine particles can be controlled, and a method of forming a Au ultrafine particle dispersed film having good reproducibility was realized.
【００１４】[0014]
【発明の効果】本発明の超微粒子分散膜の粒径制御成膜
方法は、予め超微粒子の粒径と膜厚計の表示膜厚との間
の関係を求め、膜厚計が所定の表示膜厚を示すまで、蒸
発源から蒸発した薄膜原料を基板面に蒸着させ、所定の
粒径の超微粒子よりなる分散膜を形成させるものとする
ことによって、超微粒子の粒径をコントロールすること
ができ、再現性のよい超微粒子分散膜の成膜方法を実現
する。According to the particle size control film forming method of the ultrafine particle dispersion film of the present invention, the relationship between the particle size of the ultrafine particles and the display film thickness of the film thickness meter is obtained in advance, and the film thickness meter displays the predetermined value. It is possible to control the particle size of ultrafine particles by vapor-depositing the thin film raw material evaporated from the evaporation source on the substrate surface to form a dispersion film of ultrafine particles having a predetermined particle size until the film thickness is indicated. A method for forming an ultrafine particle dispersed film that can be realized and has good reproducibility is realized.
【図１】本発明の一実施例に係る成膜装置の説明図であ
る。FIG. 1 is an explanatory diagram of a film forming apparatus according to an embodiment of the present invention.
【図２】上記一実施例に係る粒径と膜厚計表示膜厚の関
係図である。FIG. 2 is a diagram showing a relationship between a particle size and a film thickness display film thickness according to the above embodiment.
１ 真空容器 ２ ＳｉＯ2 基板 ３ 蒸発源 ４ 膜厚測定子1 vacuum container 2 SiO 2 substrate 3 evaporation source 4 film thickness gauge
Claims (1)
器中の上記基板の近傍に膜厚計の測定子を配設し、予め
膜厚計の表示膜厚と基板表面に蒸着される薄膜原料の粒
径との関係を求めた後、基板に形成される分散膜の膜厚
を上記膜厚計により測定しながら蒸発源から薄膜原料を
蒸発させ、上記予め求めた膜厚計の表示膜厚と薄膜原料
の粒径との関係より所定の粒径に対応した表示膜厚とな
るまで薄膜原料を基板に蒸着させることを特徴とする超
微粒子分散膜の粒径制御成膜方法。Claims: 1. A probe of a film thickness meter is provided in the vicinity of the substrate in a vacuum vessel having a substrate and an evaporation source provided therein, and a display film thickness of the film thickness meter is set in advance. After obtaining the relationship with the particle size of the thin film raw material deposited on the substrate surface, evaporate the thin film raw material from the evaporation source while measuring the film thickness of the dispersed film formed on the substrate with the above film thickness meter, and obtain the above in advance. Based on the relationship between the displayed film thickness of the film thickness meter and the particle size of the thin film raw material, the particle size of the ultrafine particle dispersed film is characterized in that the thin film raw material is vapor-deposited on the substrate until the displayed film thickness corresponds to the predetermined particle size. Controlled film formation method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16985391A JPH0517874A (en) | 1991-07-10 | 1991-07-10 | Formation of superfine particle dispersed film under grain size control |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16985391A JPH0517874A (en) | 1991-07-10 | 1991-07-10 | Formation of superfine particle dispersed film under grain size control |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0517874A true JPH0517874A (en) | 1993-01-26 |
Family
ID=15894153
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16985391A Withdrawn JPH0517874A (en) | 1991-07-10 | 1991-07-10 | Formation of superfine particle dispersed film under grain size control |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0517874A (en) |
-
1991
- 1991-07-10 JP JP16985391A patent/JPH0517874A/en not_active Withdrawn
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 19981008 |