JPH0283239A - Formation of dielectric thin film - Google Patents
Formation of dielectric thin filmInfo
- Publication number
- JPH0283239A JPH0283239A JP63232440A JP23244088A JPH0283239A JP H0283239 A JPH0283239 A JP H0283239A JP 63232440 A JP63232440 A JP 63232440A JP 23244088 A JP23244088 A JP 23244088A JP H0283239 A JPH0283239 A JP H0283239A
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- glass substrate
- followed
- solution
- coating
- 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
- 239000010409 thin film Substances 0.000 title claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 title description 2
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 239000011521 glass Substances 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 125000002524 organometallic group Chemical group 0.000 claims abstract 3
- 239000003960 organic solvent Substances 0.000 claims abstract 2
- 238000010438 heat treatment Methods 0.000 claims description 4
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 abstract description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 3
- 150000004703 alkoxides Chemical class 0.000 abstract description 3
- 230000001678 irradiating effect Effects 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 abstract 2
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 16
- 239000010408 film Substances 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 150000002902 organometallic compounds Chemical class 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- HHMHVPYTSZDWME-UHFFFAOYSA-N C1CCCC2=CC=CC=C12.[Ti] Chemical compound C1CCCC2=CC=CC=C12.[Ti] HHMHVPYTSZDWME-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 229940126214 compound 3 Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Landscapes
- Surface Treatment Of Optical Elements (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は誘電体薄膜の形成方法に関するものである。[Detailed description of the invention] [Industrial application field] The present invention relates to a method of forming a dielectric thin film.
公知のようにレンズ製品、フィルタ等には誘電体多層膜
がその表面にコーティングされている。As is well known, the surfaces of lens products, filters, etc. are coated with a dielectric multilayer film.
これら誘電体多層膜は真空蒸着法により形成されている
。真空蒸着法は１０−６＋ｔＯｒｒ程度の高真空で膜形
成を行なうため、スループット、コストの面で実用上大
きな問題を有していた。These dielectric multilayer films are formed by vacuum evaporation. Since the vacuum evaporation method performs film formation in a high vacuum of about 10<-6 >tOrr, it has had practical problems in terms of throughput and cost.
この解決策として例えばアプライド、オプティックス第
２４巻（１９８５年）２６６６頁から２６７３頁（Ａｐ
ｐｌｉｅｄ ０ｐｔｉｃｓ 、 ２４ 、２６６６〜２
６７３（１９８５））で述べられているよう（：有機金
属化合物をスピンナ塗布し加熱して誘電体薄膜を形成す
る方法がある。ただしこの方法では上記論文にも記述さ
れているように加熱温度を５００℃以上とする心安があ
り、高温にできない部分を含む製品には適用でさず、ま
た高温とするため製造コストを高める原因ともなる。As a solution to this problem, for example, Applied Optics Vol. 24 (1985) pp. 2666 to 2673 (Ap.
plied 0ptics, 24, 2666-2
673 (1985)), there is a method of coating an organometallic compound with a spinner and heating it to form a dielectric thin film. However, in this method, the heating temperature must be adjusted as described in the above paper. It is safe to set the temperature to 500°C or higher, but it cannot be applied to products that include parts that cannot be heated to high temperatures, and the high temperature also increases manufacturing costs.
上記従来技術は高真空を必要としない利点を有するもの
の加熱温度を５００℃以上の高温にしなければならない
という問題点があった。Although the above-mentioned conventional technology has the advantage of not requiring a high vacuum, it has the problem that the heating temperature must be raised to a high temperature of 500° C. or higher.
本発明の目的は上記問題点を解決する方法を提供するこ
とにある。An object of the present invention is to provide a method for solving the above problems.
上記目的は、有機金層化合物を塗布した後、パルス光を
照射することｄ二より達成される。The above object is achieved by applying pulsed light after applying the organic gold layer compound.
パルス光は波長１５０ｎｍ〜数μｍのものを用いること
ができ、塗布層に選択的に吸収される１ ５０ｎｍ〜４
００ｎｍの紫外光がより好適である０通常のランプをチ
ョッパを用いてパルス光としてもよいし、パルスレーザ
光により照射してもよい。The pulsed light can have a wavelength of 150 nm to several μm, and is selectively absorbed by the coating layer.
Ultraviolet light of 00 nm is more preferable.0 It is also possible to use a chopper to generate pulsed light from a normal lamp, or to irradiate with pulsed laser light.
パルスの周期は１〜１００Ｈｚの範囲で用い基板の熱伝
導率等により最適なパルス周期は異なる。The pulse period is in the range of 1 to 100 Hz, and the optimum pulse period varies depending on the thermal conductivity of the substrate, etc.
本発明の適用可能な有機金属化合物は特に限定されるも
のではないが、安全上金属アルコキシドが好適である。The organic metal compound to which the present invention can be applied is not particularly limited, but metal alkoxides are preferred for safety reasons.
形成できる誘電体膜は５ｉｎ２． ＴｉＯ□。The dielectric film that can be formed is 5in2. TiO□.
Ｓｎ ０２． Ａｔ２０． 、 Ｚｒ ０２等多岐にわ
たる。Sn 02. At20. , Zr 02, etc.
以下、本発明の実施例を図により説明する。 Embodiments of the present invention will be described below with reference to the drawings.
実施例１
金属アルコキシド（例えばチタンイソグロボキシドＴＩ
（０１−Ｃ，Ｈ，）４） ７．５重量％程度をエチレ
ングリコールモノエチルエーテルＣ２Ｈ５０ＣＨ２ＣＨ
２０Ｈに溶解し、硝酸を１重量％程度添加し塗布液とす
る。第１図に示すようにガラス基板１上：ニスピンナ回
転数５００〜３０００ ｒｐｍで上記塗布液２を塗布す
る。ランプをチョッパによりパルス化した光ａを数分間
照射し、塗布液２の加水分解反応を促進させ誘電体薄膜
６を得た。パルス光照射の際、ガラス基板１は低い温度
に保たれていたことを熱電対等によって確認した。Example 1 Metal alkoxides (e.g. titanium isogloboxide TI
(01-C,H,)4) Approximately 7.5% by weight of ethylene glycol monoethyl ether C2H50CH2CH
20H and add about 1% by weight of nitric acid to prepare a coating solution. As shown in FIG. 1, the coating liquid 2 is applied onto a glass substrate 1 using a varnish spinner at a rotational speed of 500 to 3000 rpm. The lamp was irradiated with pulsed light a using a chopper for several minutes to accelerate the hydrolysis reaction of the coating liquid 2 and obtain the dielectric thin film 6. It was confirmed using a thermocouple or the like that the glass substrate 1 was kept at a low temperature during pulsed light irradiation.
実ＩＭ列２
実施例１と同様にして塗布液をガラス基板上に塗布した
後、ＫｒＦ”ｌオシマレーザ光２４８ｎｍ （第１図の
ａ）をパルス周期１００Ｈｚで数十秒〜数分間照射した
。これにより誘電体薄膜６を得た。レーザ光照射の際、
ガラス基板１は低い温度に保たれていたことを熱電対等
によって確認した。Actual IM row 2 After coating the coating solution on a glass substrate in the same manner as in Example 1, it was irradiated with KrF''l oscillator laser light of 248 nm (a in Figure 1) at a pulse frequency of 100 Hz for several tens of seconds to several minutes. A dielectric thin film 6 was obtained.During laser light irradiation,
It was confirmed using a thermocouple or the like that the glass substrate 1 was kept at a low temperature.
また、レーザの周期を１０ Ｈｚ 〜１００ Ｈｚまで
１０Ｈｚおきに設定して同様の検討を行ないほぼ同等の
結果を得た。In addition, similar studies were conducted with the laser cycle set every 10 Hz from 10 Hz to 100 Hz, and almost the same results were obtained.
さらに、ＡｒＦ’エキシマレーザ光１９２ｎｍ 、 Ｘ
ｅａｔエキシマレーザ光５０８ｎｍ、ＸｅＦエキシマレ
ーザ光５５１ｎｍ等を用いて同様の検討を行ないほぼ同
等の結果を得た。Furthermore, ArF' excimer laser light 192 nm,
Similar studies were conducted using EAT excimer laser light of 508 nm, XeF excimer laser light of 551 nm, etc., and almost the same results were obtained.
実施例３
第２図に示すようにガラス基板１上にシリコンテトラエ
トオツド５１（ｏｃ２Ｈ５）４とチタンイソプロボキ７
ドＴｔ （ｏｉ−Ｃ５Ｈ，）４の混合物（浴媒はエチレ
ングリコールモノエチルエーテル、硝酸を１重址％添加
する）をスピンナにより塗布する。う／グをチ冒ツバに
よりパルス化した光あるいはエキシマレーザ光ａを照射
し、Ｓ ｉ Ｏ２＋ Ｔ ｘ Ｏ２層４を形成する。こ
の層の屈折率は１．７０〜１．８０とすることができた
。さらに、チタンテトライングロボキシドを用いて同様
の処理を行ないＴｉＯ□層５を形成した。この層の屈折
率は２．２〜２．０とすることができた。さらに、シリ
コンテトラエトキシドを用いて同様の処理を行ない８１
０２層６を形成した。この層の屈折率は１．４０〜１．
５０であった。Example 3 As shown in FIG.
A mixture of Tt (oi-C5H,)4 (bath medium is ethylene glycol monoethyl ether, with 1% nitric acid added) is applied using a spinner. A SiO2+TxO2 layer 4 is formed by irradiating the glass with pulsed light or excimer laser light a using a blower. The refractive index of this layer could be 1.70-1.80. Further, a similar process was performed using titanium tetraline globoxide to form a TiO□ layer 5. The refractive index of this layer could be between 2.2 and 2.0. Furthermore, similar treatment was performed using silicon tetraethoxide.81
02 layer 6 was formed. The refractive index of this layer is 1.40-1.
It was 50.
以上のようにして形成した５層膜の各層の屈折率、膜厚
を以下のように調整した。 ＳｉＯ２＋ＴｉＯ２層、屈
折率１．７４．膜Ｊ１６２０Ｘ、 ＴｌＯ２層、屈折率
２．０５、膜厚９４０Ｘ、５１層２層、屈折率１．４５
、膜厚８６０Ｘ、得られた５層膜の可視光（４５０〜６
５゜ｎｍ）ｆ二対する反射率を測定したところ、１１６
ｃｓ以下と反射防止膜として効果のあることが明らかと
なった。The refractive index and film thickness of each layer of the five-layer film formed as described above were adjusted as follows. SiO2+TiO2 layer, refractive index 1.74. Film J1620X, TlO2 layer, refractive index 2.05, film thickness 940X, 51 layers, 2 layers, refractive index 1.45
, film thickness 860X, visible light (450~6
5゜nm) When the reflectance for f2 was measured, it was 116
It became clear that the film was effective as an antireflection film when it was less than cs.
本発明によれば誘電体薄膜を高スループツト、低コスト
で形成できるので、レンズ製品、フィルタ等を安価に製
造できるという効果がある。According to the present invention, a dielectric thin film can be formed at high throughput and at low cost, so that lens products, filters, etc. can be manufactured at low cost.
第１図および第２図は本発明の実施例を示す説明図であ
る。
ａ・・・パルス光
１・・・ガラス基板
２・・・有機金属化合物を含む塗布液
３・・・誘電速薄膜
４・・・Ｓｉ Ｏ２＋Ｔｉ ０２層
５・・・ＴｌＯ２層
６・・・ＳｉＯ□層。FIG. 1 and FIG. 2 are explanatory diagrams showing an embodiment of the present invention. a...Pulsed light 1...Glass substrate 2...Coating liquid containing organometallic compound 3...Dielectric fast thin film 4...SiO2+Ti02 layer 5...TlO2 layer 6...SiO□ layer.
Claims (1)
塗布した後、加熱法としてパルス光を照射することを特
徴とする誘電体薄膜の形成方法。1. A method for forming a dielectric thin film, which comprises dissolving an organometallic complex in an organic solvent and coating the solution on a glass substrate, followed by irradiation with pulsed light as a heating method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63232440A JPH0283239A (en) | 1988-09-19 | 1988-09-19 | Formation of dielectric thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63232440A JPH0283239A (en) | 1988-09-19 | 1988-09-19 | Formation of dielectric thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0283239A true JPH0283239A (en) | 1990-03-23 |
| JPH0529617B2 JPH0529617B2 (en) | 1993-05-06 |
Family
ID=16939301
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63232440A Granted JPH0283239A (en) | 1988-09-19 | 1988-09-19 | Formation of dielectric thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0283239A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03283459A (en) * | 1990-03-30 | 1991-12-13 | Hitachi Ltd | Semiconductor integrated circuit device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57138708A (en) * | 1981-02-20 | 1982-08-27 | Hitachi Ltd | Composition for forming transparent conductive film and method of forming transparent conductive film |
-
1988
- 1988-09-19 JP JP63232440A patent/JPH0283239A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57138708A (en) * | 1981-02-20 | 1982-08-27 | Hitachi Ltd | Composition for forming transparent conductive film and method of forming transparent conductive film |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03283459A (en) * | 1990-03-30 | 1991-12-13 | Hitachi Ltd | Semiconductor integrated circuit device |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0529617B2 (en) | 1993-05-06 |
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