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JPH01308847A - Glass substrate - Google Patents

Glass substrate

Info

Publication number
JPH01308847A
JPH01308847A JP9753888A JP9753888A JPH01308847A JP H01308847 A JPH01308847 A JP H01308847A JP 9753888 A JP9753888 A JP 9753888A JP 9753888 A JP9753888 A JP 9753888A JP H01308847 A JPH01308847 A JP H01308847A
Authority
JP
Japan
Prior art keywords
glass substrate
film
glass
weather resistance
substrate
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
Application number
JP9753888A
Other languages
Japanese (ja)
Other versions
JP2509291B2 (en
Inventor
Atsunori Matsuda
厚範 松田
Shinya Katayama
慎也 片山
Yoshihiro Matsuno
好洋 松野
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Sheet Glass Co Ltd
Original Assignee
Nippon Sheet Glass Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nippon Sheet Glass Co Ltd filed Critical Nippon Sheet Glass Co Ltd
Priority to JP9753888A priority Critical patent/JP2509291B2/en
Publication of JPH01308847A publication Critical patent/JPH01308847A/en
Application granted granted Critical
Publication of JP2509291B2 publication Critical patent/JP2509291B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23Oxides
    • C03C17/25Oxides by deposition from the liquid phase
    • C03C17/256Coating containing TiO2

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

PURPOSE:To obtain a glass substrate excellent in a weather resistance by providing a specific amount of alkyl groups remaining in a calcined SiO2-TiO2-based oxide film applied to a glass substrate surface. CONSTITUTION:In a glass substrate having the surface coated with a calcined SiO2-TiO2-based oxide film prepared by calcining an alkyl group-containing organometallic compound, alkyl groups in an amount of 0.5-5wt.% based on the oxide are left in the calcined film. Although an optional glass substrate, such as soda-lime glass, borosilicate glass or aluminosilicate glass, is cited as the usable substrate, an alkaline metal-containing glass, such as the soda-lime glass, is preferably used to greatly reflect effects and reduce the cost. Any compound capable of initiating polycondensing or crosslinking reaction to increase the viscosity of solutions may be used as the above-mentioned organometallic compound. Si(OCH3)4, Ti(OC3H7)4, Zr(OC3H7)4, etc., are exemplified as the afore-mentioned compound.

Description

【発明の詳細な説明】 本発明は、耐候性の優れたガラス基板に関し、特に光磁
気ディスク基板として使用するのに優れたガラス基板に
関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a glass substrate with excellent weather resistance, and particularly to a glass substrate excellent in use as a magneto-optical disk substrate.

〔従来の技術〕[Conventional technology]

従来、絶縁膜を有するガラス基板としては、ソーダライ
ムガラス基板上に化学気相析出(CVO)法により、5
in2膜を形成したものが、広く知られている。(例え
ばN、 Goldsmitb and W、Kernt
RCA Review、 28 、 153 (196
7))また同じく化学気相析出法により5tCh  h
os系膜を形成したガラス基板が多く報告されている。
Conventionally, as a glass substrate having an insulating film, 50% was deposited on a soda lime glass substrate by a chemical vapor deposition (CVO) method.
Those in which an in2 film is formed are widely known. (e.g. N, Goldsmitb and W, Kernt
RCA Review, 28, 153 (196
7)) Also, 5tCh h by the same chemical vapor deposition method.
Many glass substrates on which OS-based films are formed have been reported.

(例えばW、 Kern、  RCA Review 
3土[4]。
(For example, W. Kern, RCA Review
3 Sat [4].

一方、溶液塗布法により絶縁膜を形成したガラス基板と
してはソーダライムガラス基板上にSiO□膜を形成し
たもの(例えば、S、 5akka、et al、。
On the other hand, as a glass substrate on which an insulating film is formed by a solution coating method, a SiO□ film is formed on a soda lime glass substrate (for example, S, 5akka, et al.

J、Non −Cryst、 5olids、63.2
23  (1984))や、SiO,−P、O,系をベ
ースとする複合酸化物膜を形成したもの(例えば特開昭
62−158136)や、Sing −TiOz系膜を
形成したもの(例えばTh1n SolidFilms
、  77129 (1981))が知られている。
J, Non-Cryst, 5olids, 63.2
23 (1984)), those with composite oxide films based on SiO, -P, O, (e.g., JP-A-62-158136), and those with Sing-TiOz-based films (e.g., Th1n). Solid Films
, 77129 (1981)) are known.

又従来、光磁気ディスク基板としては、ガラス基板上に
エツチング処理を行なうことにより凹凸を形成したもの
が知られている。(例えば、J。
Conventionally, as a magneto-optical disk substrate, a glass substrate in which irregularities are formed by etching is known. (For example, J.

Braar and K、S、Imn+ink、5PI
B、  420 206 (1983))またガラス板
の上にシリコンアルコキシドを含む溶液を塗布し型を押
しあてることにより凹凸を形成したものが知られている
。(例えば特開昭62〔発明が解決しようとする課題〕 しかしながら、上記従来のガラス基板においては高温高
湿度(例えば70℃、相対湿度90%)で保持すると、
表面にナトリウムの炭酸塩が析出したり、基板が劣化す
るという問題点があった。
Braar and K, S, Imn+ink, 5PI
B, 420 206 (1983)) It is also known to form irregularities by applying a solution containing silicon alkoxide onto a glass plate and pressing a mold against it. (For example, JP-A-62 [Problem to be Solved by the Invention]) However, when the above-mentioned conventional glass substrate is kept at high temperature and high humidity (for example, 70°C and relative humidity of 90%),
There were problems in that sodium carbonate was deposited on the surface and the substrate deteriorated.

特に高度の信転性が必要とされる光磁気ディスク1等の
基板としては、上記問題は重大な問題であった。
In particular, the above problem is a serious problem for substrates such as magneto-optical disks 1 which require a high degree of reliability.

〔課題を解決するための手段〕[Means to solve the problem]

本発明は、上記従来の問題点を解決するためになされた
ものであって、アルキル基含有金属有機化合物が焼成さ
れたSing −TiO□系酸化物焼成膜が表面に被覆
されたガラス基板において、該焼成膜に該アルキル基を
該酸化物に対して0.5〜5wt%残留させている。
The present invention has been made to solve the above-mentioned conventional problems, and includes a glass substrate whose surface is coated with a Sing-TiO□-based oxide fired film in which an alkyl group-containing metal organic compound is fired. The alkyl group is left in the fired film in an amount of 0.5 to 5 wt% based on the oxide.

本発明に使用できる基板としては、ソーダライムガラス
、ボロシリケートガラス、アルミノシリケートガラス等
任意のガラス基板が使用できるが、ソーダライムガラス
等のアルカリ金属含有ガラスを使用することが本質的に
本発明の効果が大きく反映されることになり、また価格
も低価格となるので好ましい。
As the substrate that can be used in the present invention, any glass substrate such as soda lime glass, borosilicate glass, aluminosilicate glass, etc. can be used, but it is essential to use an alkali metal-containing glass such as soda lime glass. This is preferable because the effect will be greatly reflected and the price will also be low.

本発明に用いる金属有機化合物は重縮合あるいは架橋反
応がおこることによって溶液の粘性を上昇させるような
化合物であれば使用できる。
The metal organic compound used in the present invention can be any compound that increases the viscosity of the solution by polycondensation or crosslinking reaction.

例えば5i(QC)Is)n r 5t(OCJ、)t
、 Ti(QC:)b)4゜Ti(OC4Hq)4. 
Zr(QC:+Ib)a、Zr(OCJ++)4゜八l
 (QC:1)I7)!、 Af (OCJq)*、 
Na0CJs等のN (OR)、l〔MはSi、 Ti
、 Zr、 Ca、  Aj2. Na、 Pb、  
B、 Sn。
For example, 5i(QC)Is)n r 5t(OCJ,)t
, Ti(QC:)b)4°Ti(OC4Hq)4.
Zr(QC:+Ib)a, Zr(OCJ++)4゜8l
(QC:1)I7)! , Af (OCJq) *,
N (OR) of Na0CJs, l [M is Si, Ti
, Zr, Ca, Aj2. Na, Pb,
B. Sn.

Ge等の金属、Rはメチル、エチル等のアルキル基、n
は1〜4の整数〕で示される化合物および−(J、  
−COO)l、 −COOR,−Nl(z 。
metal such as Ge, R is an alkyl group such as methyl or ethyl, n
is an integer of 1 to 4] and -(J,
-COO)l, -COOR, -Nl(z.

るいは架橋反応を行なう一般的官能基を含む金属有機化
合物等が例示できる。
Alternatively, metal organic compounds containing a general functional group that performs a crosslinking reaction can be exemplified.

ガラス基板上の前記金属有機化合物の焼成膜は、ガラス
基板を前記金属有機化合物を含む溶液(以後溶液と略称
する)に浸漬した後引き上げる方法(通称ディッピング
法)、溶液を滴下した後回転させる方法(通称スピンコ
ード法)およびスプレー法等の通常用いられている被膜
作製方法により作製された塗布膜を乾燥焼成することに
より作製される。
The fired film of the metal-organic compound on the glass substrate can be formed by immersing the glass substrate in a solution containing the metal-organic compound (hereinafter referred to as solution) and then pulling it up (commonly known as dipping method), or by dropping the solution and then rotating it. It is produced by drying and baking a coating film produced by a commonly used film production method such as a spin-coating method or a spray method.

本発明は、該金属有機化合物のSing−TiO□系の
焼成膜を該金属有機化合物のア′ルキル基が酸化物に対
して0.5〜5wt%残留したものとしているが、該焼
成膜中の残留アルキル基が5wt%よりも多いと、該焼
成膜の機械的特性が極端に低下してしまう。又残留アル
キル基が0.5wt%より少ないと、本発明の耐候性の
改善の効果が現われない。
In the present invention, the fired film of Sing-TiO If the residual alkyl group is more than 5 wt%, the mechanical properties of the fired film will be extremely reduced. Further, if the residual alkyl group is less than 0.5 wt%, the effect of improving weather resistance of the present invention will not appear.

本発明は金属有機化合物の焼成膜として、5iOz−T
iO□系膜を用いているが、該Sing−TiO□系膜
が耐候性の向上が著しい。該SiO□−TiOz系非晶
質膜の内でもSin、 −Tj(h 2成分系非晶質膜
を用いることが、製造が簡単であるので望ましい。
The present invention uses 5iOz-T as a fired film of a metal organic compound.
Although an iO□-based film is used, the Sing-TiO□-based film has significantly improved weather resistance. Among the SiO□-TiOz-based amorphous films, it is preferable to use a Sin, -Tj(h) two-component based amorphous film because it is easy to manufacture.

5in2TiO□系非晶質膜中のTie、含有量は任意
に設定できるが、6〜70モルパーセントとすることが
好ましい。該膜体のTiO□含量が6モルパーセント未
満であっても70モルパーセントを越えても、膜体を形
成したガラス基板の耐候性の向上の効果が現われにくく
なる。
The Tie content in the 5in2TiO□-based amorphous film can be set arbitrarily, but it is preferably 6 to 70 mol percent. Whether the TiO□ content of the film is less than 6 mol percent or exceeds 70 mol percent, the effect of improving the weather resistance of the glass substrate on which the film is formed is less likely to appear.

特にTi0z含有量を6〜12モルパーセントとしたも
のが、光学的な用途用基板として好ましい。
In particular, a substrate having a TiOz content of 6 to 12 mol percent is preferable as a substrate for optical applications.

該膜体のTi0z含量が6モルパーセント未満であって
も12モルパーセントを越えても、膜体とガラス基板と
の境界面における光の反射が増大しやすくなる。
Whether the Ti0z content of the film is less than 6 mol percent or exceeds 12 mol percent, light reflection at the interface between the film and the glass substrate tends to increase.

又特に、塗布膜作製溶液中に増粘剤としての有機高分子
(ポリエチレングリコール等)を含ませた様な場合には
、形成される焼成膜が気孔率の高い膜体となり、屈折率
が低下するので前記光学的用途に対するTiO2含有量
は10〜25モル%とすることが好ましい。該含有量が
10モル%未満であっても25モル%より多くとも膜体
とガラス基板との境界面における光の反射が増大しやす
い。
In addition, especially when an organic polymer (such as polyethylene glycol) is included as a thickener in the coating film preparation solution, the fired film formed will have a high porosity and the refractive index will decrease. Therefore, it is preferable that the TiO2 content for the optical use is 10 to 25 mol%. Even if the content is less than 10 mol% or more than 25 mol%, light reflection at the interface between the film and the glass substrate tends to increase.

特に光磁気ディスク基板を、前記塗布膜にプレス型等の
溝形状を転写して作製する方法においては、塗布溶液中
に増粘剤を加えておくことが作業性等の面で好ましく、
(例えば特開昭62−225273)この様な場合にお
いては前述の通りTiO2含有量を10〜25モル%と
することが好ましい。(塗布溶液中に増粘剤を加えずに
行なう場合は6〜12モル%とすることが好ましい。) 前記出発金属有機化合物のアルキル基が酸化物に対して
0.5〜5wt%残留した金属有機化合物の焼成膜は、
例えば前記金属有機化合物の塗布膜を90〜400℃の
温度で熱処理することにより得られる。
In particular, in the method of manufacturing a magneto-optical disk substrate by transferring the groove shape of a press mold or the like onto the coating film, it is preferable to add a thickener to the coating solution in terms of workability.
(For example, JP-A No. 62-225273) In such a case, the TiO2 content is preferably 10 to 25 mol % as described above. (When coating without adding a thickener to the coating solution, the concentration is preferably 6 to 12 mol %.) A metal in which the alkyl group of the starting metal organic compound remains in an amount of 0.5 to 5 wt % based on the oxide. The fired film of organic compound is
For example, it can be obtained by heat-treating the coating film of the metal organic compound at a temperature of 90 to 400°C.

90℃未満の温度の熱処理では、残留アルキル基が5w
t%以下となりに<<、又膜中に水分が多く残り、水分
に基づく問題が生じやすくなる。又前述の通り機械的強
度が低い被膜となりやすい。
In heat treatment at a temperature below 90°C, the residual alkyl group
When the amount is less than t%, a large amount of water remains in the film, and water-based problems tend to occur. Furthermore, as mentioned above, the film tends to have low mechanical strength.

400℃より高い温度の熱処理では、残留アルキル基が
0.5wt%以上となりに<<、又熱処理中に基板ガラ
ス中のアルカリ金属イオンが金属有機化合物の焼成膜中
に拡散によって入り込み、90〜400℃で焼成した被
膜による耐候性向上の効果よりもかえって低い効果しか
示さない様になりやすい。又該焼成温度は、90〜20
0℃とすることが特に良好な耐候性が得られるので望ま
しい。
In heat treatment at a temperature higher than 400°C, residual alkyl groups become 0.5 wt% or more, and alkali metal ions in the substrate glass diffuse into the fired film of the metal-organic compound during heat treatment, resulting in It tends to show only a lower effect than the effect of improving weather resistance by a film fired at ℃. Moreover, the firing temperature is 90 to 20
It is desirable to set the temperature to 0°C because particularly good weather resistance can be obtained.

該SiO□−TiO□系非晶質膜等の金属有機化合物の
焼成膜の平均膜厚は0.02〜2.0μmが好ましい。
The average film thickness of the fired film of the metal-organic compound such as the SiO□-TiO□-based amorphous film is preferably 0.02 to 2.0 μm.

咳膜体の膜厚が0.02μ1未満の場合、該膜体を設け
ることによるガラス基板の耐候性の向上の程度は低い。
When the thickness of the cough membrane body is less than 0.02μ1, the degree of improvement in weather resistance of the glass substrate due to the provision of the membrane body is low.

また該膜体の膜厚が2.0μmを越えるとはく離の問題
が生じやすくなる。
Moreover, if the film thickness of the film body exceeds 2.0 μm, peeling problems tend to occur.

特に光磁気ディスク基板として使用する場合には、該S
iO□−Tifh系非晶質膜の平均膜厚は、0.15〜
2.0μmの平均膜厚とすることが好ましい。
Especially when used as a magneto-optical disk substrate, the S
The average film thickness of the iO□-Tifh-based amorphous film is 0.15~
The average film thickness is preferably 2.0 μm.

該膜体はガラス板の両面に設けることによりガラス板の
両面を保護することができる。しかしながら、必要に応
じてガラス板の片面に設けるなど任意の形で実施できる
By providing the film on both sides of the glass plate, both sides of the glass plate can be protected. However, it can be implemented in any form, such as providing it on one side of the glass plate, if necessary.

光磁気ディスク基板として使用する場合には、ガラス基
板にエツチング法、ゾルゲルスタンプ法(特開昭62−
102445)等によって溝を形成し、その後金属有機
化合物の焼成膜を形成してもかまわない。しかしながら
、平滑なガラス基板上に表面に凹凸を存する膜体を設け
る方法が生産性が高いので好ましい。該凹凸は少なくと
も片面に設ければ良い。
When used as a magneto-optical disk substrate, the glass substrate may be etched using an etching method or a sol-gel stamping method (Japanese Patent Application Laid-Open No. 1983-1999).
102445) or the like, and then a fired film of a metal organic compound may be formed. However, a method of providing a film body having an uneven surface on a smooth glass substrate is preferable because productivity is high. The unevenness may be provided on at least one side.

上記金属有機化合物中の残留アルキル基は、例えば赤外
線分光光度法、熱重量分析法等によって測定することが
できる。
The residual alkyl group in the metal organic compound can be measured, for example, by infrared spectrophotometry, thermogravimetric analysis, or the like.

塗布に使用する溶液中に含まれる金属有機化合物のアル
キル基の量は、金属有機化合物の重合度が変化すると変
化するが、本発明で言う金属有機化合物のアルキル基の
残留量とは金属有機化合物が完全に酸化物になった場合
の重量を基準として評価している。(たとえば、原料の
Si (OCJs)が全く加水分解をうけず単量体で存
在している場合、未反応のアルキル基は酸化物Sing
の重量を基準として247wt%含まれていることにな
る。また3つのアルキル基が加水分解をうけて単量体で
存在している、即ちSi (OCzHs) (OH) 
3の形で存在している場合、未反応のアルキル基は61
wt%含まれていることになる。さらに重合度が増し、
加水分解の程度が進むと未反応のアルキル基の量は減少
する。即ちシリコン(Si)原子10個からなる無機高
分子中に未反応のエトキシ基が1個存在するような場合
、6wt%アルキル基が含まれていることになる。) 〔作 用〕 本発明によれば、該Sin、 −Tie、系金属有機化
合物の焼成膜がガラス基板側からのナトリウムイオンの
拡散防止層として作用し、該ガラス基板の耐候性を向上
させる保護膜の役割を果たしている。
The amount of alkyl groups in the metal-organic compound contained in the solution used for coating changes as the degree of polymerization of the metal-organic compound changes, but in the present invention, the residual amount of alkyl groups in the metal-organic compound refers to The evaluation is based on the weight when it completely becomes an oxide. (For example, if the raw material Si (OCJs) is not hydrolyzed at all and exists as a monomer, the unreacted alkyl group becomes the oxide Sing.
This means that it contains 247 wt% based on the weight of . In addition, three alkyl groups are present as monomers through hydrolysis, i.e., Si (OCzHs) (OH)
3, the unreacted alkyl group is 61
This means that it contains wt%. The degree of polymerization further increases,
As the degree of hydrolysis progresses, the amount of unreacted alkyl groups decreases. That is, when there is one unreacted ethoxy group in an inorganic polymer consisting of 10 silicon (Si) atoms, it means that 6 wt % of alkyl groups are contained. ) [Function] According to the present invention, the fired film of the Sin, -Tie, metal organic compound acts as a diffusion prevention layer for sodium ions from the glass substrate side, and provides protection for improving the weather resistance of the glass substrate. It plays the role of a membrane.

該金属有機化合物の焼成膜として、金属有機化合物のア
ルキル基を酸化物に対して0.5〜5wt%残留した物
を用いると、該焼成膜中のアルキル基がアルカリ金属猟
獲等の作用を行ない、良好な耐候性を実現できると考え
られる。
When using a fired film of the metal-organic compound in which 0.5 to 5 wt% of the alkyl group of the metal-organic compound remains based on the oxide, the alkyl group in the fired film will not have the effect of alkali metal hunting. It is believed that good weather resistance can be achieved by doing so.

又この様な0.5〜5wt%の残留アルキル基を有する
焼成膜は、無機骨格がすでに十分発達しており、機械的
強度を著しくそこなうことがない。
In addition, such a fired film having 0.5 to 5 wt % of residual alkyl groups already has a sufficiently developed inorganic skeleton, and its mechanical strength is not significantly impaired.

〔実施例〕〔Example〕

実施例−1 出発原料として、シリコンテトラエトキシド(Si (
OCzHs) #)およびチタニウムテトラn−ブトキ
シド(Tf(0−netHq) t)を用い、溶媒には
エタノール、加水分解触媒には塩化水素をそれぞれ用い
た。加える水の量はシリコンテトラエトキシドに対して
モル比で4倍とした。シリコンテトラエトキシドのエタ
ノール溶液に希塩酸(1wt%)を加え室温で30分間
攪拌した。その後チタニウムテトラn−ブトキシドのエ
タノール溶液を徐々に加え、同じく室温でさらに30分
間反応させた。シリコンテトラエトキシドとチタニウム
テトラn−ブトキシドはモル比で91:9となるように
した。
Example-1 Silicon tetraethoxide (Si (
OCzHs) #) and titanium tetra n-butoxide (Tf(0-netHq) t) were used, ethanol was used as a solvent, and hydrogen chloride was used as a hydrolysis catalyst. The amount of water added was 4 times that of silicon tetraethoxide in terms of molar ratio. Dilute hydrochloric acid (1 wt%) was added to an ethanol solution of silicon tetraethoxide, and the mixture was stirred at room temperature for 30 minutes. Thereafter, an ethanol solution of titanium tetra n-butoxide was gradually added, and the reaction was continued for another 30 minutes at room temperature. The molar ratio of silicon tetraethoxide and titanium tetra-n-butoxide was 91:9.

こうして得られた溶液は、黄色〜無色透明であり酸化物
換算濃度は、8.5wt%である。該溶液をエタノール
で2倍の体積に希釈して塗布溶液とした。
The solution thus obtained is yellow to colorless and transparent, and has an oxide concentration of 8.5 wt%. The solution was diluted to twice the volume with ethanol to prepare a coating solution.

該塗布溶液中にソーダライムガラス基板を浸漬し、一定
速度(1,6m/Sec )で引き上げることにより9
1Si02・9TiO□塗布膜をガラス基板上に形成し
た。該塗布膜に、迅速に峰高さ0.15μm、峰中2μ
m、峰間隔4μmの多数の峰部を有するアセチルセルロ
ース製(弾性係数10’ kg f/crA)の厚さ5
0μmの型を押しあて接合した。
By immersing a soda lime glass substrate in the coating solution and pulling it up at a constant speed (1.6 m/Sec),
A 1Si02.9TiO□ coating film was formed on a glass substrate. The coating film is quickly coated with a peak height of 0.15 μm and a peak height of 2 μm.
m, thickness 5 made of acetyl cellulose (elastic modulus 10' kg f/crA) having many peaks with a peak interval of 4 μm
Bonding was performed by pressing a 0 μm mold.

その後、離型を接合した塗布膜つきガラス基板を室温で
15分間乾燥し、次いで90℃で30分間クリーンオー
ブンを用い大気中で一次焼成を行った後アセチルロース
製の型の離型を行なった。
Thereafter, the glass substrate with the coated film bonded with the mold release was dried at room temperature for 15 minutes, and then primary baking was performed in the air using a clean oven at 90°C for 30 minutes, after which the acetylose mold was released. .

該離型後の塗布膜つきガラス基板を、400℃で15分
間最終焼成を行った。
After the mold release, the coated glass substrate was subjected to final firing at 400° C. for 15 minutes.

この最終焼成により塗布膜は平均210nm厚の非晶質
膜(M折率1.52)になっていた。
After this final baking, the coating film became an amorphous film (M refraction index: 1.52) with an average thickness of 210 nm.

上記操作により作製された光磁気ディスク基板の表面お
よび断面を走査型電子顕微鏡により観察したことろ溝深
さ約75nm、l巾副2μm、溝間隔約4μmの良好な
溝形状が形成されていた。
Observation of the surface and cross section of the magneto-optical disk substrate produced by the above procedure using a scanning electron microscope revealed that good groove shapes were formed with a groove depth of about 75 nm, a width of 2 μm, and a groove spacing of about 4 μm.

上記実施例により作製された光磁気ディスク基板の概略
断面を第1図に示す。
FIG. 1 shows a schematic cross section of the magneto-optical disk substrate manufactured according to the above embodiment.

次に該光磁気ディスク基板の耐候性試験を行った。耐候
性試験は、−旦結露させた後70℃、相対湿度90%の
雰囲気中に4日間保持することにより行った。
Next, a weather resistance test was conducted on the magneto-optical disk substrate. The weather resistance test was conducted by condensing the sample and then holding it in an atmosphere of 70° C. and 90% relative humidity for 4 days.

耐候性試験後の該光磁気ディスク基板の表面は、耐候性
試験前と同様、均一で、表面の劣化や析出物の発生は認
められなかった。
The surface of the magneto-optical disk substrate after the weather resistance test was as uniform as before the weather resistance test, and no surface deterioration or precipitation was observed.

本実施例と同一の作製方法により、最終焼成温度のみを
90℃、200℃と変えて作製した光磁気ディスク基板
について、同一の耐候性試験を行った。
The same weather resistance test was conducted on magneto-optical disk substrates manufactured by the same manufacturing method as in this example, except that the final firing temperature was changed to 90°C and 200°C.

90℃で最終熱処理したものも、200℃で最終熱処理
したものも、先の400℃で最終熱処理したものと同様
、耐候性試験後のこれらの光磁気ディスク基板の表面は
均一で表面の劣化や析出物の発生は認められなかった。
The surface of these magneto-optical disk substrates after the weather resistance test was uniform, and there was no surface deterioration, whether the final heat treatment was carried out at 90℃ or 200℃, as was the case with the final heat treatment at 400℃. No occurrence of precipitates was observed.

上記90℃、200℃、400℃の各温度で焼成した焼
成膜中の残留アルキル基を熱重量分析法により測定した
所、出発の金属有機化合物(脱水縮合前)のアルキル基
が酸化物に対して各々4.4゜3.7.0.8wt%5
iOz−TiOz系非晶質膜の組成は、上記の91Si
O□・9TiOzに限られるものではなく、木兄におい
てTiO2を6〜12モルパーセント含む組成範囲にお
いて同様の耐候性を持つ光磁気ディスク基板が得られた
When the residual alkyl groups in the fired films fired at the temperatures of 90°C, 200°C, and 400°C were measured by thermogravimetric analysis, the alkyl groups of the starting metal-organic compound (before dehydration condensation) were compared to the oxides. each 4.4゜3.7.0.8wt%5
The composition of the iOz-TiOz amorphous film is the above 91Si
The composition is not limited to O□.9TiOz, but magneto-optical disk substrates with similar weather resistance were obtained in the composition range containing 6 to 12 mole percent of TiO2.

比較例−1 表面に凹凸を存するSing −Ti0z系非晶質膜つ
きガラス基板のかわりに表面に凹凸を有するSiO□非
晶質膜つきガラス基板について実施例=1と同様の耐候
性試験を行った。
Comparative Example-1 A weather resistance test similar to Example 1 was conducted on a glass substrate with an SiO□ amorphous film having an uneven surface instead of a Sing-TiOz-based glass substrate with an amorphous film having an uneven surface. Ta.

該Sin、非晶質膜の作製方法としては、出発原料とし
てシリコンテトラエトキシドを用いた溶媒にはエタノー
ル加水分解触媒には塩化水素をそれぞれ用いた。加える
水の量およびエタノールの量はシリコンテトラエトキシ
ドに対してそれぞれ6および5とした。
In the method for producing the Sin and amorphous films, silicon tetraethoxide was used as the starting material, and hydrogen chloride was used as the solvent and ethanol hydrolysis catalyst. The amounts of water and ethanol added were 6 and 5, respectively, relative to silicon tetraethoxide.

シリコンテトラエトキシドのエタノール溶液容液に希塩
酸(1wt%)を加え室温で1時間攪拌した。
Dilute hydrochloric acid (1 wt%) was added to an ethanol solution of silicon tetraethoxide, and the mixture was stirred at room temperature for 1 hour.

こうして得られた溶液は無色透明であり、該溶液をエタ
ノールで3倍の体積に希釈して塗布溶液とした。
The solution thus obtained was colorless and transparent, and was diluted with ethanol to 3 times the volume to prepare a coating solution.

該塗布溶液を用いて実施例−1と同様の操作を行って表
面に凹凸を有するSiO□非晶質膜つきガラス基板を作
製した。400℃15分間の最終焼成により該5i(h
非晶質膜は平均200nm厚、屈折率1.45になって
いた。
Using this coating solution, the same operation as in Example 1 was carried out to prepare a glass substrate with an SiO□ amorphous film having an uneven surface. The 5i (h
The amorphous film had an average thickness of 200 nm and a refractive index of 1.45.

上記操作により作製された光磁気ディスク基板の概略断
面を第2図に示す。本比較例により作製した光磁気ディ
スク基板について実施例−1と同様の耐候性試験を行っ
た。
FIG. 2 shows a schematic cross section of the magneto-optical disk substrate produced by the above operation. The same weather resistance test as in Example 1 was conducted on the magneto-optical disk substrate produced in this comparative example.

耐候性試験後の該光磁気ディスク基板の表面には直径0
.1μfi1〜0.2μmの析出粒子が前面に1平方マ
イクロメートルあたり32ケの密度で析出していた。該
析出粒子は分析の結果ナトリウムの炭酸塩であることが
わかった。耐候性試験後の咳光磁気ディスク基板の概略
断面を第3図に示す。
After the weather resistance test, the surface of the magneto-optical disk substrate has a diameter of 0.
.. Precipitated particles of 1 μfi1 to 0.2 μm were deposited on the front surface at a density of 32 particles per 1 square micrometer. Analysis revealed that the precipitated particles were sodium carbonate. FIG. 3 shows a schematic cross section of the magneto-optical disk substrate after the weather resistance test.

本比較例と同一の作製方法により、最終焼成温度のみを
90℃、200℃と変えて作製した光磁気ディスク基板
について同一の耐候性試験を行った。
The same weather resistance test was conducted on magneto-optical disk substrates manufactured by the same manufacturing method as in this comparative example, except that the final firing temperature was changed to 90°C and 200°C.

90℃最終熱処理したものも、200℃で最終熱処理し
たものも、先の400℃で最終熱処理したものと同様、
これらの光磁気ディスク基板の表面には直径0.1〜0
.2μmの析出粒子が同程度に認められた。
The final heat treatment at 90℃ and the final heat treatment at 200℃ are the same as the final heat treatment at 400℃.
The surface of these magneto-optical disk substrates has a diameter of 0.1 to 0.
.. Precipitated particles of 2 μm were observed to the same extent.

上記90℃、200℃、400℃の各焼成膜中の残留ア
ルキル基を実施例−1と同様測定した所各々4.3 、
 4.1 、 1.1 wt%のアルキル基が酸化物(
SiO□)に対して残留していることがわかった。
The residual alkyl groups in each of the films fired at 90°C, 200°C, and 400°C were measured in the same manner as in Example-1, and the results were 4.3 and 4.3, respectively.
4.1, 1.1 wt% of alkyl groups are oxides (
It was found that it remained with respect to SiO□).

比較例−2 化学強化されたソーダライムガラス基板上にスピンコー
ド法を用いてフォトレジスト膜を形成し光磁気ディスク
基板としての溝形状に露光装置を用いて選択的に露光を
行った。現像処理を行なった後ドライエツチングによっ
て該基板上に巾約1.6μm、深さ約70nmの連続的
溝形状を作製した。フォトレジストを除去した後のガラ
ス基板の概略断面図を第4図に示す。
Comparative Example-2 A photoresist film was formed on a chemically strengthened soda lime glass substrate using a spin code method, and selectively exposed using an exposure device in the shape of a groove as a magneto-optical disk substrate. After development, a continuous groove with a width of about 1.6 μm and a depth of about 70 nm was formed on the substrate by dry etching. FIG. 4 shows a schematic cross-sectional view of the glass substrate after removing the photoresist.

上記操作により作製された光磁気ディスク基板について
実施例−1と同様の耐候性試験を行った。
The same weather resistance test as in Example 1 was conducted on the magneto-optical disk substrate produced by the above procedure.

耐候性試験後の該光磁気ディスク基板の表面は極めてひ
どい劣化をおこしており、両面ともに全面に1〜5μm
径の孔を持った網目状の析出物が観察された。
After the weather resistance test, the surface of the magneto-optical disk substrate was extremely deteriorated, with a thickness of 1 to 5 μm on both sides.
A network-like precipitate with pores of approximately 100 mm in diameter was observed.

該網目状析出物は分析の結果ナトリウムの炭酸塩である
ことがわかった。耐候性試験後の該光磁気ディスク基板
の概略断面を第5図に示す。
Analysis revealed that the network precipitate was sodium carbonate. FIG. 5 shows a schematic cross section of the magneto-optical disk substrate after the weather resistance test.

実施例−2 実施例−1で調製した塗布溶液中に平均分子量600の
ポリエチレングコール(PEG600)を、最終生成物
である91SiOz・9 TiO2組成の酸化物に対す
る重量比で(PEG600)/ (酸化物)=1の量加
え、均一に溶解したものを塗布溶液とした。
Example-2 Polyethylene glycol (PEG600) with an average molecular weight of 600 was added to the coating solution prepared in Example-1 at a weight ratio of (PEG600)/(oxidation A coating solution was prepared by adding an amount of 1% of the solution and dissolving it uniformly.

該塗布溶液を用いて実施例−1と同様の操作を行って表
面に凹凸を有するPEG600添加91SfO□・9 
TiO□非晶質膜つきガラス基板を作製した。
Using the coating solution, the same operation as in Example-1 was carried out to obtain PEG600-added 91SfO□9 having unevenness on the surface.
A glass substrate with a TiO□ amorphous film was produced.

400℃15分間の最終焼成後接布膜は平均400nm
厚の非晶質膜になっていた。また屈折率はPEG添加に
より最終焼成後;薄膜の気孔率が増大したため1.46
に低下していた。
After final firing at 400°C for 15 minutes, the average thickness of the adhered film is 400 nm.
It had become a thick amorphous film. Also, the refractive index was 1.46 after the final firing due to the addition of PEG; due to the increased porosity of the thin film.
It had declined to .

上記操作により作製された光磁気ディスク基板の表面お
よび断面を走査型電子顕微鏡により観察したところ溝深
さ69nm、溝巾約2μm、、m間隔約4μIの良好な
溝形状が形成されていた。
When the surface and cross section of the magneto-optical disk substrate produced by the above procedure was observed using a scanning electron microscope, it was found that good groove shapes were formed with a groove depth of 69 nm, a groove width of about 2 μm, and an interval of about 4 μI.

本実施例により作製した光磁気ディスク基板について実
施例−1と同様の耐候性試験を行った。
The same weather resistance test as in Example 1 was conducted on the magneto-optical disk substrate produced in this example.

耐候性試験後の該光磁気ディスク基板の表面は、耐候性
試験前と同様、均一で、表面の劣化や析出物の発生は認
められなかった。
The surface of the magneto-optical disk substrate after the weather resistance test was as uniform as before the weather resistance test, and no surface deterioration or precipitation was observed.

本実施例と同一の作製方法により、最終焼成温度のみを
90℃、200℃と変えて作製した光磁気ディスク基板
について、同一の耐候性試験を行った。
The same weather resistance test was conducted on magneto-optical disk substrates manufactured by the same manufacturing method as in this example, except that the final firing temperature was changed to 90°C and 200°C.

90℃で最終熱処理したものも、200℃で最終熱処理
したものも、先の400℃で最終熱処理したものと同様
、耐候性試験後のこれらの光磁気ディスク基板の表面は
均一で表面の劣化や析出物の発生は認められなかった。
The surface of these magneto-optical disk substrates after the weather resistance test was uniform, and there was no surface deterioration, whether the final heat treatment was carried out at 90℃ or 200℃, as was the case with the final heat treatment at 400℃. No occurrence of precipitates was observed.

上記400℃の各焼成膜中に残留する未反応アルキル基
を測定した所1.2wt%(対91SiOz:9TiO
z酸化物)であった。
The amount of unreacted alkyl groups remaining in each film fired at 400°C was measured to be 1.2wt% (vs. 91SiOz:9TiO).
z oxide).

PEG600添加5iOz  Ti0t系非晶質膜の組
成は、上記の91SiOz・9TiO□に限られるもの
ではなく木兄においてTi(hを10〜25モルパーセ
ント含む組成範囲において同様の耐候性を持つ光磁気デ
ィスク基板が得られた。特にTi0zを17モルパーセ
ント含む、PEG600を添加したこの組成の膜体は4
00℃で15分熱処理した後、屈折率1.51を有し、
膜体をガラス基板との境界面における光の反射率が少な
く優れていた。(上記83Si(h ・17TtOz4
00″C焼成膜中の残留アルキル基は酸化物に対して0
.7iyt%であった。)実施例−3 実施例−1で調製した塗布溶液中にソーダライムガラス
板を浸漬し、一定速度(1,8is / 5ec)で引
きあげ塗布膜を作製した。
The composition of the PEG600-added 5iOz Ti0t-based amorphous film is not limited to the above-mentioned 91SiOz・9TiO□. A substrate was obtained.In particular, a film body of this composition containing 17 mol percent TiOz and added with PEG600 was obtained.
After heat treatment at 00°C for 15 minutes, it has a refractive index of 1.51,
The light reflectance at the interface between the film and the glass substrate was low and excellent. (The above 83Si(h ・17TtOz4
The residual alkyl group in the 00″C fired film is 0 compared to the oxide.
.. It was 7iyt%. ) Example 3 A soda lime glass plate was immersed in the coating solution prepared in Example 1, and pulled up at a constant speed (1.8 is/5 ec) to produce a coating film.

該塗布■りつきガラス基板を090℃、30分間■20
0℃、15分間■400t15分間の熱処理を各々行っ
た。
The applied glass substrate was heated at 090°C for 30 minutes.
Heat treatment was performed at 0° C. for 15 minutes and at 400 t for 15 minutes.

90℃で熱処理した膜体の厚みは、約280nm、20
0°Cで熱処理したものは260nmおよび400℃で
熱処理したものは220nmにそれぞれなっていた。
The thickness of the film body heat-treated at 90°C is approximately 280 nm, 20
The wavelength was 260 nm for the one heat-treated at 0°C, and 220 nm for the one heat-treated at 400°C.

膜体はすべて非晶質であった。熱処理温度を変えた各ガ
ラス基板の耐候性試験を行った。
All membrane bodies were amorphous. A weather resistance test was conducted on each glass substrate at different heat treatment temperatures.

耐候性試験は、まず各ガラス基板を70℃相対湿度90
%の雰囲気中に4日間保持することにより行った。
For the weather resistance test, first, each glass substrate was heated to 70℃ relative humidity 90℃.
% atmosphere for 4 days.

本耐候性試験後の各ガラス基板の表面は、耐候性試験前
と同様均一で、表面の劣化や析出物の発生は認められな
かった。
The surface of each glass substrate after this weather resistance test was as uniform as before the weather resistance test, and no surface deterioration or precipitation was observed.

さらに各ガラス基板を一旦結露させた後、70℃相対湿
度90%の雰囲気中で4日間保持する結露試験を行った
Further, a dew condensation test was conducted in which each glass substrate was once subjected to dew condensation and then held in an atmosphere of 70° C. and 90% relative humidity for 4 days.

本結露試験後の各ガラス基板の表面は、400℃で熱処
理したものにはごくわずかに0.1μm程度の析出粒子
が認められたたものの、90℃および200℃で熱処理
したものには全く劣化や析出物は認められず、全体とし
て本方法により作製したガラス基板は極めて耐候性に優
れていることがわかった。
After this dew condensation test, the surface of each glass substrate heat-treated at 400°C showed very slight precipitated particles of about 0.1 μm, but those heat-treated at 90°C and 200°C showed no deterioration. No deposits or deposits were observed, and it was found that the glass substrate produced by this method as a whole had extremely excellent weather resistance.

また特に、該膜体を形成したガラス基板の耐候性は90
℃〜200°Cで熱処理したものが非常に優れていた。
In particular, the weather resistance of the glass substrate on which the film body is formed is 90%.
Those heat-treated at ℃ to 200℃ were very good.

実施例−4 チタニウムテトラn−ブトキシドのエタノール溶液にシ
リコンテトラエトキシドを加え、室温で20分間攪拌し
た後、濃塩酸(36wt%)を加え、同じく室温で20
分間反応させた。次に全金属アルコキシドに対してモル
比で4倍となるように不足の水を加えさらに同しく室温
で20分間攪拌を続けた。
Example-4 Silicon tetraethoxide was added to an ethanol solution of titanium tetra-n-butoxide, stirred at room temperature for 20 minutes, concentrated hydrochloric acid (36 wt%) was added, and the mixture was stirred for 20 minutes at room temperature.
Allowed to react for minutes. Next, an insufficient amount of water was added so that the molar ratio was 4 times that of all the metal alkoxides, and stirring was continued for 20 minutes at room temperature.

チタニウムテトラn−ブトキシドとシリコンテトラエト
キシドのモル比は70:30となるようにした。
The molar ratio of titanium tetra n-butoxide and silicon tetraethoxide was set to 70:30.

こうして得られた溶液をエタノールで4倍の体積に希釈
して塗布溶液とした。
The solution thus obtained was diluted with ethanol to 4 times the volume to prepare a coating solution.

3g ?g液を用いて実施例■と同様の操作を行って3
0SiO,・70TiQ2塗布膜をソーダライム板上に
形成した。
3g? Perform the same operation as in Example ① using liquid g to obtain 3.
A coating film of 0SiO,.70TiQ2 was formed on a soda lime board.

該塗布膜つきガラス基板を実施例−4と同様■90℃で
30分間、0200℃で15分間、0400°Cで15
分間の熱処理を各々行った。
The glass substrate with the coating film was heated in the same manner as in Example-4.
Each heat treatment was performed for 1 minute.

90℃で熱処理した該膜体の厚みは約240nm、20
0℃で熱処理したものは210nmおよび400℃で熱
処理したものは180nn+にそれぞれなっていた。
The thickness of the film body heat-treated at 90°C is about 240 nm, 20
Those heat-treated at 0°C had a diameter of 210 nm, and those heat-treated at 400°C had a diameter of 180 nn+.

膜体はすべて非晶質であった。又90℃、200”C,
400℃の各温度での焼成膜中の残留アルキル基を測定
した所与々4.2. 3.9. 0.6wt%(対30
StO,・70TiO,酸化物)であった。
All membrane bodies were amorphous. Also 90℃, 200"C,
4.2. Residual alkyl groups in the fired film were measured at various temperatures of 400°C. 3.9. 0.6wt% (vs. 30
StO, 70TiO, oxide).

上記実施例により作製されたガラス基板について実施例
−1と同様の耐候性試験および結露試験を行った。
The same weather resistance test and dew condensation test as in Example-1 were conducted on the glass substrate produced in the above example.

その結果本実施例により作製された3QStO□・70
TiO,非晶質膜つきガラス基板は先の実施例−〇で述
べた9 1SiO,・9 Ti1t非晶質膜つきガラス
基板同様、試験後表面の劣化や析出物は認められず、耐
候性に優れていることがわかった。また90℃〜200
℃で熱処理したものが耐候性の点においては特に優れて
いた。
As a result, 3QStO□・70 produced according to this example
As with the glass substrate with the TiO, amorphous film described in the previous example-〇, no surface deterioration or precipitates were observed after the test, and the weather resistance was improved. I found it to be excellent. Also 90℃~200℃
Those heat-treated at ℃ were particularly excellent in terms of weather resistance.

SiO□−TiO□系非晶質膜の組成は、上記実施例−
4、および実施例5の915t(h ・9 TiChあ
るいは、30SiO□・70TiOtに限られるもので
はなく、来県においてTiO□を6〜70モルパーセン
ト含む組成範囲において同様の耐候性を持つガラス基板
が得られた。
The composition of the SiO□-TiO□-based amorphous film is the same as in the above example-
4, and 915t (h 9 TiCh or 30SiO□ 70TiOt in Example 5, but in the next prefecture, there are glass substrates with similar weather resistance in the composition range containing 6 to 70 mole percent TiO□. Obtained.

比較例−3 膜体を有さないソーダライムガラス板について実施例−
4と同様の耐候性試験を行った。
Comparative Example-3 Example of soda lime glass plate without film body-
A weather resistance test similar to that in 4 was conducted.

70℃相対湿度90%で4日間保持した後の膜体を有し
ない該ガラス基板の表面は掻めてひどい劣化をおこして
おり、全面に1〜7μm径の孔を持った網目状析出物や
直径0.2〜0.4μmの析出粒子が観察された。
After being held at 70°C and 90% relative humidity for 4 days, the surface of the glass substrate without a film was scratched and severely deteriorated, and the entire surface was covered with network-like precipitates with pores of 1 to 7 μm in diameter. Precipitated particles with a diameter of 0.2 to 0.4 μm were observed.

これらの析出物は、分析結果、ナトリウムの炭酸塩であ
ることがわかった。
As a result of analysis, these precipitates were found to be sodium carbonate.

SiO□−Tie、系非晶質膜つきガラス基板のかわり
にSiO□非晶質膜つきガラス基板について実施例−3
と同様の耐候性試験を行った。
Example-3 of glass substrate with SiO□ amorphous film instead of SiO□-Tie, glass substrate with system amorphous film
A weather resistance test similar to that was conducted.

実施例2で調製した塗布溶液を用いて実施例−3と同様
の操作を行ってSiO□塗布膜をソーダライムガラス板
上に形成した。
Using the coating solution prepared in Example 2, the same operation as in Example 3 was performed to form a SiO□ coating film on a soda lime glass plate.

該塗布膜つきガラス基板を■90℃30分間■200℃
で15分間■400℃で15分間の熱処理を各々行った
The glass substrate with the coating film is heated to ■90℃ for 30 minutes■200℃
Heat treatment was performed at 400° C. for 15 minutes and at 400° C. for 15 minutes, respectively.

90℃で熱処理した膜体の厚みは、約280nm。The thickness of the film body heat-treated at 90°C is approximately 280 nm.

200℃で熱処理したものは260nmおよび400℃
で熱処理したものに230nmにそれぞれなっていた。
260nm and 400℃ for those heat treated at 200℃
The wavelength was 230 nm after heat treatment.

膜体はすべて非晶質であった。All membrane bodies were amorphous.

本比較例により作製したガラス基板について、実施例−
3と同様の耐候性試験を行った。
Regarding the glass substrate produced according to this comparative example, Example-
A weather resistance test similar to No. 3 was conducted.

結露試験後の該ガラス基板の表面には直径0.1〜0.
2μmの析出粒子が全面に析出していた。
The surface of the glass substrate after the dew condensation test has a diameter of 0.1 to 0.
Precipitated particles of 2 μm were deposited over the entire surface.

また粒子の析出量は、熱処理温度の高いものほど多く、
特に400℃で熱処理した試料には2〜4μmの幅の筋
状析出物が全面に観察された。
In addition, the amount of particles precipitated increases as the heat treatment temperature increases;
In particular, streak-like precipitates with a width of 2 to 4 μm were observed over the entire surface of the sample heat-treated at 400°C.

これらの析出物は、分析の結果ナトリウムの炭酸塩であ
ることがわかった。
Analysis revealed that these precipitates were sodium carbonate.

上記実施例および比較例により作製されたガラス基板お
よびその他のガラス基板の耐候性および焼成膜中の残留
アルキル基(対最終酸化物)を第1表に示す。
Table 1 shows the weather resistance of the glass substrates and other glass substrates produced in the above Examples and Comparative Examples and the residual alkyl groups in the fired films (versus the final oxide).

第1表中の耐候性は耐候性試験後のガラス基板の表面を
走査型電子顕微鏡(SEM)ですべて検査し、評価した
ものであって、◎印は耐候性良好を示し順次◎〉○〉△
>x>xx>xxxxと悪化を示し××××印は耐候性
劣悪を示す。
The weather resistance in Table 1 was evaluated by inspecting the surface of the glass substrate after the weather resistance test using a scanning electron microscope (SEM), and the ◎ mark indicates good weather resistance, and the order is ◎〉○〉 △
>x>xx>xxxx indicates deterioration, and XXXX indicates poor weather resistance.

金属有機化合物を出発原料とするアルキル基残留焼成膜
つきガラス基板は、上記表より明らかなように金属有機
化合物を500℃以上の温度で焼成したガラス基板や、
膜体を存さないガラス基板にくらべて非常に耐候性の点
において優れている。
As is clear from the table above, glass substrates with alkyl group residual fired films using metal-organic compounds as starting materials include glass substrates with metal-organic compounds fired at a temperature of 500°C or higher,
It has excellent weather resistance compared to glass substrates that do not have a film.

本発明の金属有機化合物の低温焼成によって得られる膜
体付ガラス基板は、光磁気ディスク用基板のみならず、
エレクトロルミネッセンス素子、エレクトロクロミック
素子、液晶素子等の表示素子や薄膜トランジスター等の
電子部品を形成するガラス基板としても適用することが
できる。また、光学部品などに本膜体を形成して、その
耐環境性を向上させることができる。
The film-attached glass substrate obtained by low-temperature firing of the metal-organic compound of the present invention can be used not only as a substrate for magneto-optical disks, but also as a substrate for magneto-optical disks.
It can also be applied as a glass substrate for forming display elements such as electroluminescent elements, electrochromic elements, and liquid crystal elements, and electronic components such as thin film transistors. Furthermore, the film body can be formed on optical components and the like to improve their environmental resistance.

〔発明の効果〕〔Effect of the invention〕

本発明のガラス基板は、実施例、比較例がらも明らかな
とうり、従来法によって作製したガラス基板に比べ耐候
性において非常に優れている。そのため従来法のガラス
基板よりも、信頼性の高い基板として使用することがで
きる。
As is clear from the Examples and Comparative Examples, the glass substrate of the present invention is extremely superior in weather resistance compared to glass substrates produced by conventional methods. Therefore, it can be used as a more reliable substrate than conventional glass substrates.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は実施例−1で作製した光磁気ディスク基板の概
略を示す断面図、第2図は比較例−1で作製した光磁気
ディスク基板の概略を示す断面図および第3図は比較例
−1で作製した光磁気ディスク基板の耐候性試験後の概
略を示す断面図である。また第4図は比較例−2で作製
した光磁気ディスク基板の概略を示す断面図、および第
5図は比較例−2で作製した光磁気ディスク基板の耐候
性試験後の概略を示す断面図である。 第1図 第2図 第3図 第5図 手  続  補  正  書 / 事件の表示 特願昭63−97538号 特公昭  −号 J0発明の名称 ガラス基板 3 補正をする者 事件との関係 特許出願人 住 所 大阪府大阪市東区道修町4丁目8番地名 称 
(lθθ)日本板硝子株式会社代表者  利 賀 信 
雄 グ代理人 7、補正の内容 (1)l’JII吉1頁20行目に「C■0」とあるの
を「CVDJと補正する。 (2)明細N4頁11行目にrN(OR)。」とあるの
をrM(OR)。」と補正する。 (3)明細書10頁16行目に「猟獲等」とあるのを「
捕獲等」と補正する。 (4)明細書12頁16行目に「溝巾副」とあるのを「
満巾約」と補正する。 (5)明m1113頁20行目にro、8wt%SiO
2」とあるのをro、8wt%残留していることがわか
った。5iO2Jと補正する。 (6)明細書14頁11行目に「用いた溶媒に」とある
のを「用いた。溶媒に」と補正する。 (7)明細!14頁14行目に「それぞれ6」とあるの
を「それぞれモル比で6」と補正する。 (8)明1114iF15頁11行目に「前面」とある
のを「全面」と補正する。 (9)明細jiF21頁17行目に「実施例■」とある
のを「実施例−3」と補正する。 (10)明細書21頁18行目に「ソーダライム板上に
」とあるのを「ソーダライムガラス基板上に」と補正す
る。 (11)明細1F22頁16行目に「■で」とあるのを
「3」と補正する。 (12)明細fi23頁2行目に「実施例5」とあるの
を「実施例−5」と補正する。
Fig. 1 is a cross-sectional view schematically showing the magneto-optical disk substrate manufactured in Example-1, Fig. 2 is a cross-sectional view schematically showing the magneto-optical disk substrate fabricated in Comparative Example-1, and Fig. 3 is a comparative example. FIG. 2 is a cross-sectional view schematically showing the magneto-optical disk substrate manufactured in Example 1-1 after a weather resistance test. Further, FIG. 4 is a cross-sectional view schematically showing the magneto-optical disk substrate manufactured in Comparative Example-2, and FIG. 5 is a cross-sectional view schematically showing the magneto-optical disk substrate manufactured in Comparative Example-2 after a weather resistance test. It is. Figure 1 Figure 2 Figure 3 Figure 5 Procedures Amendment/Indication of Case Patent Application No. Sho 63-97538 Patent Publication No. J0 Name of Invention Glass Substrate 3 Person making the amendment Relationship to the case Patent applicant Address: 4-8 Doshomachi, Higashi-ku, Osaka-shi, Osaka Name:
(lθθ) Shin Toga, Representative of Nippon Sheet Glass Co., Ltd.
Yugu Agent 7, contents of amendment (1) l'JIIKichi, page 1, line 20, "C ■ 0" is corrected to "CVDJ." (2) Specification N, page 4, line 11, rN(OR ).” is rM(OR). ” he corrected. (3) On page 10, line 16 of the specification, the phrase “games, etc.” was replaced with “
``Capture, etc.'' (4) On page 12, line 16 of the specification, the phrase “ditch width sub” should be changed to “
``Full breadth contract'' is corrected. (5) ro, 8wt%SiO on page 20 of Akira m1113
It was found that 8 wt % of RO remained in the column labeled ``2''. Correct it to 5iO2J. (6) On page 14, line 11 of the specification, the phrase "in the solvent used" is corrected to "in the solvent used." (7) Details! On page 14, line 14, "6 for each" is corrected to "6 for each in molar ratio." (8) In the 11th line of page 1114iF15, the word "front" is corrected to "full surface." (9) In the 17th line of page 21 of the specification, "Example ■" is corrected to "Example-3." (10) On page 21, line 18 of the specification, the phrase "on a soda lime board" is corrected to "on a soda lime glass substrate." (11) In the 16th line of page 22 of Specification 1F, correct "■ in" to "3". (12) In the second line of page 23 of the specification, "Example 5" is corrected to "Example-5."

Claims (3)

【特許請求の範囲】[Claims] (1)アルキル基含有金属有機化合物が焼成されたSi
O_2−TiO_2系酸化物焼成膜が表面に被覆された
ガラス基板において、該焼成膜に該アルキル基を該酸化
物に対して0.5〜5wt%残留させたことを特徴とす
るガラス基板。
(1) Si in which an alkyl group-containing metal organic compound is fired
A glass substrate whose surface is coated with a fired film of O_2-TiO_2-based oxide, characterized in that the fired film has the alkyl group remaining in an amount of 0.5 to 5 wt% based on the oxide.
(2)該焼成膜が90〜400℃の温度の焼成膜である
請求項1記載のガラス基板。
(2) The glass substrate according to claim 1, wherein the fired film is fired at a temperature of 90 to 400°C.
(3)該焼成膜が表面に凹凸を有する膜体である請求項
1又は2記載のガラス基板。
(3) The glass substrate according to claim 1 or 2, wherein the fired film is a film body having an uneven surface.
JP9753888A 1988-01-21 1988-04-20 Glass substrate Expired - Fee Related JP2509291B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP9753888A JP2509291B2 (en) 1988-01-21 1988-04-20 Glass substrate

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP63-11238 1988-01-21
JP1123888 1988-01-21
JP9753888A JP2509291B2 (en) 1988-01-21 1988-04-20 Glass substrate

Publications (2)

Publication Number Publication Date
JPH01308847A true JPH01308847A (en) 1989-12-13
JP2509291B2 JP2509291B2 (en) 1996-06-19

Family

ID=26346652

Family Applications (1)

Application Number Title Priority Date Filing Date
JP9753888A Expired - Fee Related JP2509291B2 (en) 1988-01-21 1988-04-20 Glass substrate

Country Status (1)

Country Link
JP (1) JP2509291B2 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03242843A (en) * 1990-01-31 1991-10-29 Internatl Business Mach Corp <Ibm> Magneto-optic storage medium and dielectric layer thereof
US7811684B2 (en) 2005-02-18 2010-10-12 Canon Kabushiki Kaisha Optical transparent member and optical system using the same
US8501270B2 (en) 2005-02-18 2013-08-06 Canon Kabushiki Kaisha Optical transparent member and optical system using the same

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03242843A (en) * 1990-01-31 1991-10-29 Internatl Business Mach Corp <Ibm> Magneto-optic storage medium and dielectric layer thereof
US7811684B2 (en) 2005-02-18 2010-10-12 Canon Kabushiki Kaisha Optical transparent member and optical system using the same
US7931936B2 (en) 2005-02-18 2011-04-26 Canon Kabushiki Kaisha Optical transparent member and optical system using the same
US8501270B2 (en) 2005-02-18 2013-08-06 Canon Kabushiki Kaisha Optical transparent member and optical system using the same

Also Published As

Publication number Publication date
JP2509291B2 (en) 1996-06-19

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