JPH04124257A - Method for adjusting color of tio film by ion plating - Google Patents
Method for adjusting color of tio film by ion platingInfo
- Publication number
- JPH04124257A JPH04124257A JP24389490A JP24389490A JPH04124257A JP H04124257 A JPH04124257 A JP H04124257A JP 24389490 A JP24389490 A JP 24389490A JP 24389490 A JP24389490 A JP 24389490A JP H04124257 A JPH04124257 A JP H04124257A
- Authority
- JP
- Japan
- Prior art keywords
- evaporation
- substrate
- vacuum chamber
- evaporating
- hollow cathode
- 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.)
- Granted
Links
- 238000007733 ion plating Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 67
- 230000008020 evaporation Effects 0.000 claims abstract description 57
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 24
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 5
- 229910001882 dioxygen Inorganic materials 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 6
- 239000003086 colorant Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 20
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、ホローカソードイオンプレーティング法によ
り表面にＴｉＯ膜を形成した耐蝕、耐摩耗性を有する装
飾材に於いて、再現性良く複数種の色彩をＴｉＯ膜に施
す色彩調整方法に関する。Detailed Description of the Invention (Industrial Application Field) The present invention is directed to a decorative material having corrosion and abrasion resistance that has a TiO film formed on its surface by a hollow cathode ion plating method. The present invention relates to a color adjustment method for applying a color to a TiO film.
（従来の技術）
従来よりホローカソード蒸発源の蒸発容器に収容した蒸
発材をホローカソード電子銃からの電子ビームにより溶
解蒸発させ、その蒸発物をイオンプレーティング電源に
接続した基板に付着させるイオンプレーティング法は知
られている。(Prior art) Conventionally, ion plating involves melting and evaporating the evaporation material housed in the evaporation container of a hollow cathode evaporation source using an electron beam from a hollow cathode electron gun, and depositing the evaporation material on a substrate connected to an ion plating power supply. The ting method is known.
この方法で該基板にＴｉＯ膜を形成する場合、該蒸発容
器内にＴｉを収容し、該真空室内をｌロー４〜１Ｏ−７
Ｔｏｒｒの高真空に排気してからホローカソード電子銃
を介してＡｒガスを流し乍ら該電子銃に電力を投入する
。これにより該電子銃に発生する熱電子が蒸発容器内の
蒸発材を電子衝撃し、該蒸発材が溶解する。そしてイオ
ンプレーティング電源を作動させて基板に高電圧を印加
すると共に真空室内に０２ガスを設定圧力まで導入する
と、蒸発容器から蒸発するＴ１の蒸気とＯ２が反応して
基板に耐蝕性、耐摩耗性の良１．）Ｔｉ。When forming a TiO film on the substrate using this method, Ti is stored in the evaporation container and the vacuum chamber is
After evacuation to a high vacuum of Torr, power is supplied to the electron gun while flowing Ar gas through the hollow cathode electron gun. As a result, the thermoelectrons generated by the electron gun impact the evaporation material in the evaporation container, and the evaporation material is dissolved. Then, when the ion plating power supply is activated to apply a high voltage to the substrate and 02 gas is introduced into the vacuum chamber up to the set pressure, the T1 vapor evaporated from the evaporation container and O2 react, making the substrate corrosion-resistant and wear-resistant. Good sex 1. )Ti.
膜が形成される。A film is formed.
（発明が解決しようとする課題）
ＴｉＯ膜がもつ耐蝕、耐摩耗性は、装飾用の膜として好
都合であるが、膜の色彩をコントロールすることが困難
で、真空室内に導入される０２ガスの分圧を制御するこ
とにより色彩を複数種に変化させることも考えたが、Ｔ
ｔの蒸発速度が変わったり、真空室内の残留ガスの度合
の変化などが生じるため色彩の再現性が得られないこと
がわかった。(Problems to be Solved by the Invention) The corrosion and abrasion resistance of the TiO film makes it advantageous as a decorative film, but it is difficult to control the color of the film, and it is difficult to control the color of the 02 gas introduced into the vacuum chamber. I thought about changing the color into multiple types by controlling the partial pressure, but T
It has been found that color reproducibility cannot be obtained because the evaporation rate of t changes or the degree of residual gas in the vacuum chamber changes.
本発明は、イオンプレーティング法により形成されるＴ
ｉＯ膜に、琥珀色、黄色、茶色、青色等の色彩を再現性
よく着色してその装飾性を向上させることを目的とする
ものである。The present invention provides T
The purpose of this invention is to color an iO film with colors such as amber, yellow, brown, and blue with good reproducibility to improve its decorative properties.
（課題を解決するための手段）
本発明では、上記目的を達成するために、真空室内に、
蒸発容器とホローカソード電子銃で構成されるホローカ
ソード蒸発源と、該蒸発容器の上方にイオンプレーティ
ング用電源に接続した基板とを用意し、該蒸発容器に収
めたＴｊの蒸発材料をホローカソード電子銃により酸素
雰囲気中で溶融蒸発させて該基板にＴｉＯの薄膜を形成
する方法に於いて、該蒸発源に投入する電力又は電流と
真空室内の酸素ガスの流量の割合を調整して該基板に堆
積するＴｉＯ膜に着色を施すようにした。(Means for Solving the Problems) In the present invention, in order to achieve the above object, in a vacuum chamber,
A hollow cathode evaporation source consisting of an evaporation container and a hollow cathode electron gun, and a substrate connected to an ion plating power source above the evaporation container are prepared, and the Tj evaporation material contained in the evaporation container is transferred to the hollow cathode. In the method of forming a thin film of TiO on the substrate by melting and evaporating it in an oxygen atmosphere with an electron gun, the substrate is heated by adjusting the ratio of the power or current input to the evaporation source and the flow rate of oxygen gas in the vacuum chamber. The TiO film deposited on the substrate was colored.
（作 用）
蒸発容器内に蒸発材料としてＴ１を用意し、真空室内を
高真空に排気したのちホローカソード電子銃からＡ「ガ
スを流し乍ら該電子銃に蒸発用の電力を投入すると、ホ
ローカソード法による熱電子が該電子銃から蒸発容器内
の蒸発材料Ｔ１を電子衝撃し、該蒸発材料Ｔｊか溶解す
る。そして、イオンプレーティング電源を入れると共に
真空室内に０２ガスを導入する。こうした作用は従来の
イオンプレーティング法と同様であり、基板の表面には
耐蝕性、耐摩耗性の良いＴｉＯ膜か形成されるが、本発
明の場合、電子銃に投入される蒸発用電源の電力又は電
流と０２ガスの流量との割合を制御するもので、この制
御によりその割合が小さいときは灰色になり、割合が大
きくなるにつれ青色から茶色、更に黄色になり、やがて
琥珀色になる。(Function) Prepare T1 as an evaporation material in an evaporation container, evacuate the vacuum chamber to a high vacuum, and then supply A gas from a hollow cathode electron gun while supplying evaporation power to the electron gun. Thermionic electrons generated by the cathode method impact the evaporation material T1 in the evaporation container with electrons from the electron gun, and the evaporation material Tj is dissolved.Then, the ion plating power is turned on and 02 gas is introduced into the vacuum chamber.These effects is similar to the conventional ion plating method, and a TiO film with good corrosion resistance and wear resistance is formed on the surface of the substrate. It controls the ratio between the current and the flow rate of the 02 gas, and when the ratio is small, the color becomes gray, and as the ratio increases, the color changes from blue to brown, then yellow, and eventually becomes amber.
従って、この割合が一定になるように蒸発源の電力又は
電流と０□の流量の何れか一方或いは両方を制御すれば
一定の色彩を再現することができる。Therefore, if one or both of the power or current of the evaporation source and the flow rate of 0□ are controlled so that this ratio is constant, a constant color can be reproduced.
（実施例）
本発明の実施に使用した装置を第１図に基づき説明する
と、符号（１）は真空排気口（２）と真空計（３）及び
酸素ガス導入口（４）を備えた真空室を示し、該真空室
（１）内に、下方のＴ１の蒸発材料（５）を収めた蒸発
容器（６）と側方のホローカソード電子銃（７）とで構
成された公知のホローカソード蒸発源（８）が設けられ
る。該蒸発容器り６）は導電性の材料で形成され、アー
スに接続される。また、該ホローカソード蒸発源（８）
には蒸発用電源（９）と放電用Ａｒガスの導入管（ｌＯ
）が接続され、該導入管（１０）からＡ「ガスを流し乍
ら蒸発用電源（９）の電力を投入すると、ホローカソー
ド電子銃（７）と蒸発容器（６゛）との間で放電が発生
し、該電子銃（７）から蒸発容器（６）に向けて熱電子
が放射されて蒸発材料（５）が溶解される。(Example) The apparatus used in carrying out the present invention will be explained based on FIG. A known hollow cathode is shown in the vacuum chamber (1), which is composed of an evaporation container (6) containing a lower T1 evaporation material (5) and a lateral hollow cathode electron gun (7). An evaporation source (8) is provided. The evaporation vessel 6) is made of an electrically conductive material and is connected to ground. In addition, the hollow cathode evaporation source (8)
is equipped with an evaporation power source (9) and an Ar gas introduction tube for discharge (lO
) is connected, and when the evaporation power source (9) is turned on while flowing gas A from the introduction tube (10), a discharge occurs between the hollow cathode electron gun (7) and the evaporation container (6゛). is generated, thermionic electrons are emitted from the electron gun (7) toward the evaporation container (6), and the evaporation material (5) is melted.
該真空室（１）の上方には、蒸発容器（６）と対向して
イオンプレーティング電源（１１）に接続された基板ホ
ルダ（１２）が設けられ、該基板ホルダ（１２）に装飾
用原材料の基板（１３）が取り付けられる。Above the vacuum chamber (1), a substrate holder (12) facing the evaporation container (6) and connected to an ion plating power source (11) is provided, and a decorative raw material is placed in the substrate holder (12). A board (13) is attached.
以上の構成を有するイオンプレーティング装置は、従来
のものと変わりがなく、該基板（１３）にイオンプレー
ティングによりＴｉＯ膜を形成する場合、該真空室（１
）内を１０−’ 〜１．０−’Ｔｏｒｒの高真空に排気
し、ホローカソード電子銃（７）に導入管（１０）から
Ａｒガスを流し乍ら該電子銃（７）に蒸発用電源（９）
から電力を投入する。これにより該電子銃（７）から熱
電子が蒸発容器（６）内の蒸発材料（５）を電子衝撃し
、該蒸発材料が溶解する。続いてイオンプレーティング
電源（１１）から基板（１３）に高電圧を印加すると共
に真空室（１）内に０２ガスを設定圧力まで導入すると
、蒸発容器（６）から蒸発するＴｊの蒸気と０２か反応
して基板（１３）に耐蝕性、耐摩耗性の良いＴｉＯ膜が
形成されることも従来の場合と変わりがない。The ion plating apparatus having the above configuration is the same as the conventional one, and when forming a TiO film on the substrate (13) by ion plating, the vacuum chamber (1
) was evacuated to a high vacuum of 10-' to 1.0-' Torr, and while flowing Ar gas from the introduction tube (10) into the hollow cathode electron gun (7), an evaporation power source was connected to the electron gun (7). (9)
Power is supplied from As a result, thermionic electrons from the electron gun (7) impact the evaporation material (5) in the evaporation container (6), causing the evaporation material to melt. Next, when a high voltage is applied to the substrate (13) from the ion plating power source (11) and 02 gas is introduced into the vacuum chamber (1) up to the set pressure, Tj vapor and 02 gas evaporate from the evaporation container (6). It is no different from the conventional case that a TiO film having good corrosion resistance and wear resistance is formed on the substrate (13) by the reaction.
本発明の方法では、基板（１３）に形成されるＴｉＯ膜
の色彩を調節し、しかも確実な再現性を得るために、該
蒸発源（８）に投入する電力又は電流と真空室（１）内
の酸素ガスの流量の割合を調整して該基板に堆積するＴ
ｉＯ膜を着色するもので、その具体的実施例は次の通り
である。In the method of the present invention, in order to adjust the color of the TiO film formed on the substrate (13) and to obtain reliable reproducibility, electric power or current is applied to the evaporation source (8), and the vacuum chamber (1) is The T deposited on the substrate by adjusting the flow rate of oxygen gas in
The iO film is colored, and specific examples thereof are as follows.
真空室（１）内を１０−’ 〜１０−’Ｔｏｒｒの高真
空に排気したのち、ホローカソード電子銃（７）に導入
管（１０）からＡｒガスを流し乍ら該電子銃（７）に蒸
発用電源（９）から５．５Ｋｗの一定の電力を投入する
。そして該電子銃（ア）からの熱電子の衝撃で蒸発材料
（５）を溶解させ、ＤＣ電源から成るイオンプレーティ
ング電源（１１）から２５０℃に加熱した基板（１３）
に−２０Ｖの高電圧を印加し、真空室（１）内にマスフ
ローコントローラーで制御しなから０２ガス導入口（４
）から０゜ガスを導入し、その０２の流量を２００〜１
．２００８ＣＣＨの間で可変できるようにした。After evacuating the inside of the vacuum chamber (1) to a high vacuum of 10-' to 10-' Torr, Ar gas was flowed into the hollow cathode electron gun (7) from the introduction tube (10) and the electron gun (7) was evacuated. A constant power of 5.5 Kw is supplied from the evaporation power source (9). Then, the evaporation material (5) is melted by the bombardment of thermionic electrons from the electron gun (A), and the substrate (13) is heated to 250°C by an ion plating power source (11) consisting of a DC power source.
A high voltage of -20V is applied to the vacuum chamber (1), and the 02 gas inlet (4
) 0° gas is introduced, and the flow rate of 02 is set to 200~1
．． It was made variable between 2008CCH.
そして、該蒸発用電源（９）の電力と０２ガスの流量の
割合を２８に設定すると琥珀色のＴｉＯ膜が基板（１３
）に形成され、その割合を４．６に設定すると灰色のＴ
ｉＯ膜か基板（１３）に形成された。Then, when the ratio of the power of the evaporation power source (9) and the flow rate of the 02 gas is set to 28, the amber TiO film is coated on the substrate (13).
), and if you set the ratio to 4.6, the gray T
An iO film was formed on the substrate (13).
またその割合を２８から次第に小さく設定すると、形成
されるＴｆＯ膜は乳白色、黄色、薄茶色、茶色、淡青、
更には青色に変わり、その割合を設定すれば所望の色彩
の膜を繰り返し基板（１３）に形成できた。第２図に蒸
発用電源（９）の電力と０□ガスの割合と色彩の関係を
示す。この図に於いて、Ｌ８は１００段階で表わされた
明度、ａｌの（＋）表示は赤、（−）表示は緑を表わし
、ｂｌの（＋）表示は黄、（−）表示は青を表わす。If the ratio is set gradually smaller from 28, the TfO film formed will be milky white, yellow, light brown, brown, light blue,
Furthermore, it turned blue, and by setting the proportion, it was possible to repeatedly form a film of a desired color on the substrate (13). Figure 2 shows the relationship between the power of the evaporation power source (9), the proportion of 0□ gas, and the color. In this figure, L8 is the brightness expressed in 100 steps, the (+) indication of al is red, the (-) indication is green, the (+) indication of bl is yellow, and the (-) indication is blue. represents.
酸素ガスの流量を一定とし、蒸発源の電力を可変制御し
てもＴｉＯ膜を再現性良く着色することが出来る。Even if the flow rate of oxygen gas is kept constant and the power of the evaporation source is variably controlled, the TiO film can be colored with good reproducibility.
（発明の効果）
以上のように、本発明においては、イオンプレーティン
グ法により形成されるＴＩＯ膜の色彩を、ホローカソー
ド蒸発源に投入する電力又は電流と０２ガスの流量との
割合を調節するようにしたので、基板に堆積するＴｉＯ
膜の色彩を複数種に変化させ且つ再現性良く調整するこ
と力（出来、例えばメガネフレームや時計）くンド等の
装飾品に好都合に適用できる等の効果がある。(Effects of the Invention) As described above, in the present invention, the color of the TIO film formed by the ion plating method is adjusted by adjusting the ratio of the electric power or current input to the hollow cathode evaporation source and the flow rate of the 02 gas. As a result, the TiO deposited on the substrate
It has the effect of being able to change the color of the film into multiple types and adjusting it with good reproducibility (for example, it can be conveniently applied to ornaments such as eyeglass frames and watches) and accessories.
第１図は本発明の実施に使用した装置の裁断側面図、第
２図は蒸発源の電力と０２ガスの流量との割合とＴｉＯ
膜の色彩との関係を示す線図である。
（１）・・・真空室 ＜４）・・・酸素ガス導入口（
５）・・・蒸発材料 （６）・・・蒸発容器（７）・・
・ホローカソード電子銃
（８）・・・ホローカソード蒸発源
（９）・・・蒸発用電源
（１１）・・・イオンブレーティ
ング用電源
（１３）・・
基
板
外３名Figure 1 is a cut-away side view of the device used to carry out the present invention, and Figure 2 shows the ratio of the power of the evaporation source to the flow rate of 02 gas and the TiO2 gas flow rate.
FIG. 3 is a diagram showing the relationship with the color of the film. (1)...Vacuum chamber <4)...Oxygen gas inlet (
5)...Evaporation material (6)...Evaporation container (7)...
・Hollow cathode electron gun (8)...Hollow cathode evaporation source (9)...Evaporation power source (11)...Ion blating power source (13)...3 people outside the board
Claims (1)
れるホローカソード蒸発源と、該蒸発容器の上方にイオ
ンプレーティング用電源に接続した基板とを用意し、該
蒸発容器に収めたＴｉの蒸発材料をホローカソード電子
銃により酸素雰囲気中で溶融蒸発させて該基板にＴｉＯ
の薄膜を形成する方法に於いて、該蒸発源に投入する電
力又は電流と真空室内の酸素ガスの流量の割合を調整し
て該基板に堆積するＴｉＯ膜に着色することを特徴とす
るイオンプレーティングによるＴｉＯ膜の色彩調整方法
。A hollow cathode evaporation source consisting of an evaporation container and a hollow cathode electron gun, and a substrate connected to an ion plating power source above the evaporation container are prepared in a vacuum chamber, and the Ti contained in the evaporation container is evaporated. TiO is deposited on the substrate by melting and evaporating the material in an oxygen atmosphere using a hollow cathode electron gun.
In the method for forming a thin film, the ion spray method is characterized in that the TiO film deposited on the substrate is colored by adjusting the ratio of the electric power or current input to the evaporation source and the flow rate of oxygen gas in the vacuum chamber. A method for adjusting the color of a TiO film by tinting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2243894A JP2525279B2 (en) | 1990-09-17 | 1990-09-17 | Color adjustment method of TiO film by ion plating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2243894A JP2525279B2 (en) | 1990-09-17 | 1990-09-17 | Color adjustment method of TiO film by ion plating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04124257A true JPH04124257A (en) | 1992-04-24 |
| JP2525279B2 JP2525279B2 (en) | 1996-08-14 |
Family
ID=17110580
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2243894A Expired - Fee Related JP2525279B2 (en) | 1990-09-17 | 1990-09-17 | Color adjustment method of TiO film by ion plating |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2525279B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04235274A (en) * | 1991-01-11 | 1992-08-24 | Sanyo Electric Co Ltd | Method for forming high functional thin film |
-
1990
- 1990-09-17 JP JP2243894A patent/JP2525279B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04235274A (en) * | 1991-01-11 | 1992-08-24 | Sanyo Electric Co Ltd | Method for forming high functional thin film |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2525279B2 (en) | 1996-08-14 |
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