JPS6151281B2 - - Google Patents
Info
- Publication number
- JPS6151281B2 JPS6151281B2 JP57011245A JP1124582A JPS6151281B2 JP S6151281 B2 JPS6151281 B2 JP S6151281B2 JP 57011245 A JP57011245 A JP 57011245A JP 1124582 A JP1124582 A JP 1124582A JP S6151281 B2 JPS6151281 B2 JP S6151281B2
- Authority
- JP
- Japan
- Prior art keywords
- deposited film
- weight
- sintered body
- tio
- sio
- 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
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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Physical Vapour Deposition (AREA)
Description
【発明の詳細な説明】
本発明は電子ビーム加熱によつて真空蒸着する
際に蒸発源として使用される新規な焼結体、特に
反射防止膜、保護膜として使用される蒸着膜を得
るための蒸発源物質に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention is a novel sintered body used as an evaporation source in vacuum deposition by electron beam heating, particularly for obtaining a deposited film used as an antireflection film or a protective film. Regarding evaporation source substances.
最近、真空蒸着の際、蒸発源物質を加熱するの
に電子ビーム加熱が採用されている。これは、従
来の抵抗加熱では、高融点の物質例えばTiO2が
溶解し難く、そのため蒸着が難しいことによる。 Recently, electron beam heating has been employed to heat the source material during vacuum deposition. This is because conventional resistance heating does not easily dissolve high melting point substances such as TiO 2 and therefore makes it difficult to deposit them.
ところで反射防止膜や保護膜として多用されて
いるものの中で低屈折率物質として代表的なもの
はSiO2で、他方高屈折率物質として代表的なも
のはTiO2であり、これらを混合すれば混合比に
応じて両者の中間の所望の屈折率を有する蒸膜率
を作ることができる。 By the way, among the materials that are often used as anti-reflection films and protective films, SiO 2 is a typical low refractive index material, while TiO 2 is a typical high refractive index material, and if these are mixed, Depending on the mixing ratio, a vapor deposition rate having a desired refractive index between the two can be created.
しかしながら、SiO2とTiO2粉末混合物を電子
ビーム加熱により蒸発させると、蒸発源物質が小
さな塊となつて飛びはねる現象がみられ、そのた
め蒸着膜中に小さな塊（当業者はこれをブツとい
う）が生じ、商品価値のない蒸着膜が得られる。 However, when a SiO 2 and TiO 2 powder mixture is evaporated by electron beam heating, a phenomenon is observed in which the evaporation source material becomes small lumps and scatters, resulting in small lumps (referred to as "bubbles" by those skilled in the art) in the deposited film. occurs, resulting in a deposited film with no commercial value.
そこで本発明者が研究した結果、金属モリブテ
ン粉末の添加がその“飛びはね”現象の抑制に著
効があることを見い出した。 As a result of research conducted by the present inventor, it has been found that the addition of metal molybdenum powder is extremely effective in suppressing the "splatter" phenomenon.
しかしながら、SiO2、TiO2及び金属モリデン
（Mo）の粉末混合物を蒸発源として電子ビーム加
熱により真空蒸着すると、蒸着膜が不均質にな
り、そのため安定した光学定数（屈折率・吸収係
数）を得ることが難しく、実用化は無理であるこ
とが判つた。 However, when a powder mixture of SiO 2 , TiO 2 , and metal molydene (Mo) is vacuum-deposited by electron beam heating using a powder mixture as an evaporation source, the deposited film becomes non-uniform, which makes it difficult to obtain stable optical constants (refractive index and absorption coefficient). It turned out to be difficult and impossible to put into practical use.
本発明者は、更に研究を進めた結果、それらの
粉末混合物をプレス成形した後、真空焼結したも
のは、均質な蒸着膜を与え、蒸着膜の光学定数が
安定することを見い出し、本発明を成すに至つ
た。 As a result of further research, the present inventor found that press-molding the powder mixture and then sintering it in vacuum gives a homogeneous deposited film and stabilizes the optical constants of the deposited film. We have achieved this goal.
従つて、本発明はSiO2、TiO2及び金属Moから
なる電子ビーム加熱真空蒸着用焼結体を提供す
る。 Therefore, the present invention provides a sintered body for electron beam heating vacuum evaporation consisting of SiO 2 , TiO 2 and metal Mo.
本発明の焼結体に於いて、SiO2は20〜90重量
％、TiO2は10〜80重量％（粉末混合物を固める
為には10重量％以上必要であり、蒸着膜が均質で
あり、安定した光学定数を得る為には80重量％以
下であるを必要とする）、金属Moは0.5〜50重量
％（１重量％以上にすると褐色に着色した蒸着膜
が得られる）を占めるが適当である。 In the sintered body of the present invention, SiO 2 is 20 to 90% by weight, TiO 2 is 10 to 80% by weight (more than 10% by weight is required to solidify the powder mixture, and the deposited film is homogeneous. In order to obtain stable optical constants, it is necessary to have a content of 80% by weight or less), and the metal Mo accounts for 0.5 to 50% by weight (if it is more than 1% by weight, a brown colored vapor deposited film is obtained), but it is appropriate. It is.
この焼結体を製造するためには、各成分粉末を
プレス圧１〜20t/cm2で所望の形状例えば直方体
（25×25×15mm）にプレス成形した後、800〜1500
℃、10-1〜10-5Torrの雰囲気中で真空焼結する。 In order to manufacture this sintered body, each component powder is press-molded into a desired shape, for example, a rectangular parallelepiped (25 x 25 x 15 mm) at a press pressure of 1 to 20 t/ cm2 , and then
℃, vacuum sintering in an atmosphere of 10 -1 to 10 -5 Torr.
こうして得られる本発明の焼結体は、電子ビー
ム加熱による真空蒸着に使用されるが、ブツのな
い無色又は褐色の透明で安定した光学定数を有す
る均質な蒸着膜を与える。 The thus obtained sintered body of the present invention is used for vacuum deposition by electron beam heating, and provides a homogeneous deposited film that is clear, colorless or brown, and has stable optical constants.
次いで、実施例により本発明を具体例に説明す
る。 Next, the present invention will be specifically explained with reference to Examples.
実施例 １
SiO2、TiO2金属Moの重量％比47.6：47.6：4.8
からなる粉末混合物を５t/cm2のプレス圧でプレス
成形した後、1250℃、10-3Torrで６時間真空焼
結することにより、25×25×15mmの焼結体を得
た。Example 1 Weight % ratio of SiO 2 and TiO 2 metal Mo 47.6:47.6:4.8
A sintered body of 25 x 25 x 15 mm was obtained by press-molding the powder mixture consisting of the following at a press pressure of 5 t/cm 2 and vacuum sintering at 1250°C and 10 -3 Torr for 6 hours.
この焼結体を蒸着源として
真空度：５×10-5Torr
基板温度：200℃
蒸着速度：厚さ1/4λ／30秒
の条件にてガラス板上に蒸着すると、ブツのない
平滑で透明な蒸着膜（光学的膜厚1/4λ：λ＝
500nｍ）が得られた。 Using this sintered body as a deposition source, the vacuum level: 5×10 -5 Torr, substrate temperature: 200℃, deposition rate: thickness 1/4λ/30 seconds is deposited on a glass plate, and the result is smooth and transparent without any blemishes. Deposited film (optical film thickness 1/4λ: λ=
500 nm) was obtained.
この蒸着膜は屈折率1.64で褐色に着色してお
り、500nｍの光の透過吸収率は３％であつた。 This vapor-deposited film was colored brown with a refractive index of 1.64, and the transmission/absorption rate of light at 500 nm was 3%.
実施例 ２
実施例１と同様に、SiO2：41.7重量％、
TiO2：41.7重量％、金属Mo16.6重量％からなる
焼結体を作り、蒸着を行なつたところ、ブツのな
い平滑で褐色の蒸着膜（光学的膜厚1/4λ：λ＝
500nｍ）が得られた。この蒸着膜は屈折率1.83
で、500nｍの光の透過吸収率は10％であつた。Example 2 Similar to Example 1, SiO 2 :41.7% by weight,
When a sintered body consisting of TiO 2 :41.7% by weight and metal Mo16.6% by weight was made and vapor-deposited, a smooth brown vapor-deposited film with no bumps (optical film thickness 1/4λ: λ=
500 nm) was obtained. This vapor deposited film has a refractive index of 1.83.
The transmission/absorption rate of light at 500 nm was 10%.
Claims (1)
デンからなる電子ビーム加熱真空蒸着用焼結体。1 A sintered body for electron beam heating and vacuum deposition consisting of silicon dioxide, titanium dioxide, and metal molybdenum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57011245A JPS58130275A (en) | 1982-01-27 | 1982-01-27 | Sintered body for vacuum deposition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57011245A JPS58130275A (en) | 1982-01-27 | 1982-01-27 | Sintered body for vacuum deposition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58130275A JPS58130275A (en) | 1983-08-03 |
| JPS6151281B2 true JPS6151281B2 (en) | 1986-11-08 |
Family
ID=11772550
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57011245A Granted JPS58130275A (en) | 1982-01-27 | 1982-01-27 | Sintered body for vacuum deposition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58130275A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63192857A (en) * | 1987-02-05 | 1988-08-10 | Sumitomo Electric Ind Ltd | Method for producing superconducting thin films |
-
1982
- 1982-01-27 JP JP57011245A patent/JPS58130275A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58130275A (en) | 1983-08-03 |
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