JPH03112806A - Production of coating film of silicon dioxide and device therefor - Google Patents
Production of coating film of silicon dioxide and device thereforInfo
- Publication number
- JPH03112806A JPH03112806A JP24965789A JP24965789A JPH03112806A JP H03112806 A JPH03112806 A JP H03112806A JP 24965789 A JP24965789 A JP 24965789A JP 24965789 A JP24965789 A JP 24965789A JP H03112806 A JPH03112806 A JP H03112806A
- Authority
- JP
- Japan
- Prior art keywords
- silicon dioxide
- liquid
- solution
- processing
- tank
- 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 60
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 59
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 238000000576 coating method Methods 0.000 title abstract description 9
- 239000011248 coating agent Substances 0.000 title abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 16
- 238000003860 storage Methods 0.000 claims abstract description 8
- 238000007654 immersion Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 83
- 238000002156 mixing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical class O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 1
- 229910052681 coesite Inorganic materials 0.000 abstract 4
- 229910052906 cristobalite Inorganic materials 0.000 abstract 4
- 229910052682 stishovite Inorganic materials 0.000 abstract 4
- 229910052905 tridymite Inorganic materials 0.000 abstract 4
- 239000000243 solution Substances 0.000 description 32
- 238000000034 method Methods 0.000 description 19
- 230000015572 biosynthetic process Effects 0.000 description 11
- 239000002245 particle Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012047 saturated solution Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野］
本発明は二酸化珪素被膜の製造方法及び装置に関し、特
に二酸化珪素の珪弗化水素酸溶液への溶解度の温度依存
性を利用した珪弗化水素酸の二酸化珪素過飽和溶液と基
材とを接触させて基材表面に二酸化珪素被膜を製造する
方法及び装置の改良法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method and apparatus for producing a silicon dioxide coating, and in particular to a silicofluorination process that utilizes the temperature dependence of the solubility of silicon dioxide in a hydrosilicofluoric acid solution. The present invention relates to a method for producing a silicon dioxide film on the surface of a substrate by contacting the substrate with a supersaturated silicon dioxide solution of hydrogen acid, and an improved method for the apparatus.
［従来の技術］
二酸化珪素被膜形成方法として、真空蒸着、スパッター
ＣＶＤ、浸漬塗布法（ディッピング法）のほか、装置
が簡便でありかつ大きな基材への二酸化珪素被膜形成が
可能な方法として二酸化珪素が過飽和状態となった珪弗
化水素酸溶液を含む処理液に基材を浸漬して基材表面に
二酸化珪素被膜を析出させる方法（以後析出法と呼ぶ）
が知られている。（例えば特開昭６Ｏ−３３２３３）ま
た析出法のうち特に廃液処理の必要がな（ひいては製造
コストが低いという利点を有する、二酸化珪素の珪弗化
水素酸溶液への溶解度の温度依存性を利用した珪弗化水
素酸の二酸化珪素飽和溶液を含む処理液に基材を浸漬す
る方法（特開昭６ｌ−２８１０４７）およびその方法に
適した二酸化珪素被膜の製造装置（実開昭６３−１０２
７３８）が知られている。[Prior Art] In addition to vacuum evaporation, sputter CVD, and dip coating methods as methods for forming silicon dioxide films, silicon dioxide is also used as a method that uses simple equipment and can form silicon dioxide films on large substrates. A method in which a silicon dioxide film is deposited on the surface of the substrate by immersing the substrate in a treatment solution containing a supersaturated hydrosilicofluoric acid solution (hereinafter referred to as the precipitation method)
It has been known. (For example, JP-A-6O-33233) Also, among the precipitation methods, there is no need for waste liquid treatment (therefore, the manufacturing cost is low), and the temperature dependence of the solubility of silicon dioxide in a hydrosilicofluoric acid solution is utilized. A method of immersing a substrate in a treatment solution containing a silicon dioxide saturated solution of hydrosilicofluoric acid (Japanese Unexamined Patent Publication No. 61-281047) and a manufacturing apparatus for a silicon dioxide coating suitable for the method (Utility Model Application No. 63-102)
738) is known.
上記の二酸化珪素被膜製造装置は、基材を浸漬する処理
槽と処理液調合槽、処理液予備加熱槽からなり、処理液
はこれら３つの槽の間を循環され、常に二酸化珪素が過
飽和状態となった処理液を処理槽内に導入することによ
り長時間にわたり連続的かつ安定した速度で被膜の製造
を行うことができる。さらにその経路途中に設けられた
フィルターにて粒子を濾過し、析出速度を早めても平滑
な表面を持つ被膜を得ることができる。The above-mentioned silicon dioxide coating production apparatus consists of a processing tank in which the substrate is immersed, a processing liquid mixing tank, and a processing liquid preheating tank.The processing liquid is circulated between these three tanks to ensure that silicon dioxide is always in a supersaturated state. By introducing the resulting treatment liquid into the treatment tank, the film can be manufactured continuously and at a stable rate over a long period of time. Furthermore, even if the particles are filtered through a filter provided in the middle of the path and the deposition rate is accelerated, a film with a smooth surface can be obtained.
［発明が解決しようとする問題点］
しかし上記の製造装置は、フィルターによる粒子の濾過
と処理液の調合を１つの循環経路で行うため、循環され
る処理液の全量（処理槽内の処理液１に対し３％／ｗｉ
ｎ以上）を−旦冷却し二酸化珪素を飽和溶解してから再
度加熱しなければならず、加熱及び冷却に要する費用が
高くなりひいては被膜の製造コストが高くなるといった
欠点があった。[Problems to be Solved by the Invention] However, in the above-mentioned manufacturing apparatus, the filtration of particles by the filter and the preparation of the processing liquid are carried out in one circulation path. 3%/wi for 1
n or more) must be cooled once to saturately dissolve the silicon dioxide and then heated again, which has the drawback of increasing the cost required for heating and cooling, which in turn increases the manufacturing cost of the coating.
［問題点を解決するための手段］
本発明は上記の問題点を解決するために、二酸化珪素が
略飽和状態となった珪弗化水素酸溶液の溶液温度を上昇
させて得られる二酸化珪素が過飽和状態である珪弗化水
素酸溶液を含む処理液と基材とを接触させて基材表面に
二酸化珪素を析出させる二酸化珪素被膜の製造方法およ
び装置において、溶液温度を上昇させることにより二酸
化珪素が過飽和状態となった処理槽内の処理液に対し、
低温において二酸化珪素が略飽和状態である珪弗化水素
酸溶液を添加し処理槽内の処理液中の二酸化珪素を過飽
和状態に保つことにより、長期に渡り安定した速度で二
酸化珪素被膜を製造する方法およびその方法に適した装
置を提供するものである。[Means for Solving the Problems] In order to solve the above-mentioned problems, the present invention aims to solve the above problems by increasing the temperature of a hydrosilicofluoric acid solution in which silicon dioxide is substantially saturated. In a method and apparatus for producing a silicon dioxide film, in which silicon dioxide is deposited on the surface of a substrate by contacting a treatment solution containing a supersaturated hydrofluorosilicic acid solution with a substrate, silicon dioxide is deposited by increasing the temperature of the solution. For the processing liquid in the processing tank that has become supersaturated,
A silicon dioxide film is produced at a stable rate over a long period of time by adding a hydrosilicofluoric acid solution in which silicon dioxide is almost saturated at low temperatures and keeping the silicon dioxide in the processing solution in the processing tank in a supersaturated state. A method and apparatus suitable for the method are provided.
ここで略飽和状態とは完全な飽和状態及びほぼ飽和に近
い状態を含めた言葉であり、本発明において略飽和状態
としては、完全飽和状態であることが好ましい。Here, the term "substantially saturated state" includes a completely saturated state and a nearly saturated state, and in the present invention, the substantially saturated state is preferably a completely saturated state.
この方法において処理槽内の処理液を一定量に保つため
、添加された処理液と同量を処理槽から排出することが
必要である。また、平滑な表面を持つ被膜を得るため上
記に示した処理液添加の経路とは別に、処理液源適用に
メツシュ径が１．５μｍ以下のフィルターを備えた経路
を設け１分あたりに処理槽内の処理液量の３％以上を循
環する必要かある。In this method, in order to maintain a constant amount of processing liquid in the processing tank, it is necessary to discharge the same amount of processing liquid from the processing tank as added processing liquid. In addition, in order to obtain a film with a smooth surface, in addition to the treatment liquid addition route shown above, a route equipped with a filter with a mesh diameter of 1.5 μm or less was installed to apply the treatment liquid source, and the treatment tank It is necessary to circulate more than 3% of the amount of processing liquid in the tank.
ここで、添加される処理液の温度ＴＩは３５°Ｃ以下で
あり、処理槽内の処理液温度Ｔ２は７０″Ｃ以下であり
、処理槽内の処理液温度と添加さｈる処理液温度との差
（Ｔ２−ＴＩ）は１０℃尊上であることが処理液からの
四弗化珪素蒸気の発生の抑制による処理液濃度変化の低
減や二酸化珪素被膜形成速度の点から好ましい。Here, the temperature TI of the processing liquid to be added is 35°C or less, the temperature T2 of the processing liquid in the processing tank is 70"C or less, and the temperature of the processing liquid in the processing tank and the temperature of the processing liquid to be added are It is preferable that the difference (T2-TI) is 10° C. or higher from the viewpoint of reducing the change in concentration of the processing solution by suppressing the generation of silicon tetrafluoride vapor from the processing solution and the rate of silicon dioxide film formation.
また処理液の添加速度は速い方が、珪弗化水素酸溶液に
溶解した二酸化珪素を多（処理槽内に供給することにな
るので、より高い成膜速度が得られる。ただし、１分あ
たりに添加される処理液の量が処理槽内の処理液量に対
して１．２％以上となると、成膜速度は上昇せず、製造
コストが高くなるだけであるので好ましくない。この理
由に関してはよく分かっていないが、処理液の添加量の
増加と共に処理槽内の二酸化珪素が過飽和状態である処
理液の排出ｍも多くなるためと予想される。In addition, the faster the addition rate of the treatment liquid, the more silicon dioxide dissolved in the hydrosilicofluoric acid solution will be supplied into the treatment tank, resulting in a higher film formation rate. If the amount of processing liquid added to the processing liquid is 1.2% or more with respect to the amount of processing liquid in the processing tank, it is not preferable because the film formation rate will not increase and the manufacturing cost will only increase.Regarding this reason. Although not well understood, it is expected that as the amount of the treatment liquid added increases, the amount of discharge m of the treatment liquid in which the silicon dioxide in the treatment tank is supersaturated also increases.
また処理液の添加は連続あるいは不連続でもかまわない
が、不連続に添加した場合には処理液中に溶解する二酸
化珪素の濃度分布が起こり、高濃度の部分にて二酸化珪
素の粒子が発生し易くなるので好ましくない。Furthermore, the treatment liquid may be added continuously or discontinuously, but if it is added discontinuously, the concentration distribution of silicon dioxide dissolved in the treatment liquid will occur, and silicon dioxide particles will be generated in areas with high concentration. This is not preferable because it makes it easier.
本発明に用いる珪弗化水素酸の二酸化珪素略飽和溶液は
、例えば珪弗化水素酸溶液に二酸化珪素（例えば工業用
シリカゲル、石英ガラス等）を溶解することで得られる
。また珪弗化水素酸の−ｒａ Ｗは任意のものが使用で
きるが、１モル／Ｑ以上の濃度が工業的に使用できる速
さの析出速度が得られるので好ましい。尚、３モル／＄
１より高濃度の場合には四弗化珪素蒸気の発生が激しく
なり被膜の成膜速度の低下を導くが、気液の界面を制御
することにより解消可能である。The substantially saturated solution of silicon dioxide in hydrofluorosilicic acid used in the present invention can be obtained, for example, by dissolving silicon dioxide (eg, industrial silica gel, quartz glass, etc.) in a hydrofluoric silicic acid solution. Further, any -ra W of hydrosilicic acid can be used, but a concentration of 1 mol/Q or more is preferable since a precipitation rate that is industrially usable can be obtained. In addition, 3 mol/$
When the concentration is higher than 1, silicon tetrafluoride vapor is generated intensely, leading to a decrease in the film formation rate, but this can be solved by controlling the gas-liquid interface.
［作用］
本発明は、二酸化珪素の珪弗化水素酸溶液への溶解度の
温度依存性を利用した二酸化珪素被膜の製造方法および
装置において、処理槽内の温度上昇により二酸化珪素の
過飽和状態となった処理液に対して、低温において二酸
化珪素が略胞和状態である処理液を１分あたりに処理槽
内の処理液全量の１．２ｘ以下を添加するだけで工業的
に使用可能な成膜速度を得られることを見いだすことに
よりなされた。[Function] The present invention provides a method and apparatus for producing a silicon dioxide film that utilizes the temperature dependence of the solubility of silicon dioxide in a hydrosilicofluoric acid solution. Film formation that can be used industrially by simply adding 1.2x or less of the total amount of processing solution in the processing tank per minute to the processing solution in which silicon dioxide is in a substantially hydrated state at low temperatures. This was done by finding that speed could be obtained.
この方法により、長期間にわたり連続的にかつ安定した
成膜速度で被膜の製造を安価にて行うことができる。ま
た、処理液の添加の際に同時に排出された処理液を冷却
し二酸化珪素の飽和溶解を行うことにより、再度添加用
の処理液として用いることができ、さらに製造コストを
下げることが可能である。By this method, it is possible to manufacture a film continuously and at a stable film formation rate over a long period of time at low cost. In addition, by cooling the treatment liquid discharged at the same time as the addition of the treatment liquid and performing saturated dissolution of silicon dioxide, it can be used again as a treatment liquid for addition, further reducing manufacturing costs. .
［実施例１］
処理液調合槽（１）にて−３°Ｃの温度で２モル、１１
度の珪弗化水素酸に二酸化珪素（工業用シリカゲル）を
飽和溶解して処理液を調合し、得られた処理液全量を送
液ポンプ（１２Ａ）にて送液管（１１Ａ）を通し処理液
保存槽（２）に送液した。この際濾過フィルター（１３
Ａ）にて、処理液を調合した際に溶は残った二酸化珪素
粒子を濾過した。[Example 1] 2 mol, 11 at a temperature of -3°C in the treatment liquid mixing tank (1)
A treatment solution is prepared by dissolving silicon dioxide (industrial silica gel) in saturated hydrofluorosilicic acid, and the entire amount of the obtained treatment solution is passed through the solution pipe (11A) using the solution pump (12A) for treatment. The liquid was sent to the liquid storage tank (2). At this time, the filtration filter (13
In A), the silicon dioxide particles remaining in the solution when the treatment solution was prepared were filtered.
次に送液ポンプ（１２Ｂ）にて送液管（１１Ｂ）を通し
処理液保存槽内の処理液を、処理槽（３）の整流部（９
）へ１．７２送液した。送液後、送液ポンプ（１２Ｄ）
にて送液管（１１Ｄ）を通し処理ｄυ ル カ１ＴＩ１
１ｔｆ１６）；’に’ｎｎＷ ／ ＋ ｎ
Ｓ す１％ Ｓ、力ｆｌＴ甲 −ｔｒ＋ ＊
＊ 棟へ１７０Ｊ／１Ｉｌｉｎの速度で循環を開始
しその経路途中に設けられたフィルター（１３Ｂまたは
１３Ｃ）ｉこて処理液を濾過するとともに、ヒーター（
６）にて処理槽内の処理液を加熱し６０°Ｃに昇温及び
その温度で保持した。Next, the processing liquid in the processing liquid storage tank is passed through the liquid sending pipe (11B) by the liquid sending pump (12B) to the rectifier (9) of the processing tank (3).
) was sent for 1.72 hours. After liquid feeding, liquid feeding pump (12D)
Pass the liquid through the liquid sending pipe (11D) at
1tf16);'to'nnW/+n
S 1% S, forceflTko -tr+ *
* It starts circulating to the ridge at a speed of 170J/1Ilin, and a filter (13B or 13C) installed in the middle of the route filters the trowel treatment liquid, and also a heater (
In step 6), the treatment liquid in the treatment tank was heated to 60°C and maintained at that temperature.
また、それと同時に送液ポンプ（１２Ｂ）にて処理液を
処理液保存槽からそれぞれ５．１０．２０．３０ｍ２／
ｍ１ｎ（これらは処理槽内の処理液量に対しそれぞれ０
．３．０．６． ！、 ２．１．８％／ｍｉｎに該当す
る）の速度で処理槽の添加部（ｌＯ）に添加し、同時に
送液ポンプ（１２Ｃ）にてそれぞれ添加と同じ速度で処
理槽の浸漬部のオーバーフロ一部より処理液を送液管（
１１Ｃ）を通し処理液調合槽へ排出した。排出された処
理液を処理液調合槽にて再度冷却し二酸化珪素を飽和溶
解した。処理液調合槽、処理液保存槽そして処理槽間の
処理液の送液は、以後被膜の製造を終了するまで行った
。At the same time, the treatment liquid is pumped from the treatment liquid storage tank to 5, 10, 20, 30 m2/
m1n (each of these is 0 for the amount of processing liquid in the processing tank)
．． 3.0.6. ! , corresponding to 2.1.8%/min) to the addition section (lO) of the processing tank, and at the same time, the liquid feed pump (12C) was used to overflow the immersion section of the processing tank at the same rate as the addition. The processing liquid is sent from the flow part through the liquid pipe (
11C) and was discharged to the treatment liquid mixing tank. The discharged treatment liquid was cooled again in the treatment liquid mixing tank to dissolve silicon dioxide to saturation. The processing solution was transferred between the processing solution mixing tank, the processing solution storage tank, and the processing tanks until the production of the coating was completed.
二酸化珪素被膜を成膜させる基材には２５ｍｍＸ ２５
ｍｍの７リフンウエハーを用い、処理液の加熱開始から
１時間毎に浸ｔｊシ、各々の基材上に成膜した二酸化珪
素被膜の膜厚から成膜速度の経時変化を調べた。The base material on which the silicon dioxide film is to be formed is 25 mm x 25
Using a 7-mm thick wafer, the wafer was immersed every hour from the start of heating the treatment solution, and the change in film formation rate over time was investigated from the thickness of the silicon dioxide film formed on each substrate.
上記の方法によって得られた被膜の２４時間の平均成膜
速度の結果を第１表に示す。Table 1 shows the average deposition rate over 24 hours of the coatings obtained by the above method.
第 １ 表
この結果より従来のように循環される処理液全量（処理
槽内の処理液量の３％以上）を冷却し二酸化珪素を飽和
溶解しなくても、１分あたりに処理槽内の処理液全量の
１．２％以下の世を添加するだけで、工業用に用いるの
に十分な成膜速度が得られることが分かる。Table 1 The results show that even if silicon dioxide is not saturated and dissolved by cooling the entire amount of circulating processing liquid (more than 3% of the amount of processing liquid in the processing tank) as in the conventional method, the amount of water in the processing tank per minute increases. It can be seen that by adding 1.2% or less of the total amount of the treatment solution, a film formation rate sufficient for industrial use can be obtained.
［実施例２コ
実施例１と同様の方法にて二酸化珪素被膜の製造を行な
った。尚、処理液の添加はｌｏｍＱ／ｍｉｎ （処理槽
内の処理液量に対し０．６％／ｗｉｎ）の速さで７２時
間行なった。[Example 2] A silicon dioxide coating was produced in the same manner as in Example 1. The treatment liquid was added at a rate of lomQ/min (0.6%/win relative to the amount of treatment liquid in the treatment tank) for 72 hours.
上記の方法において、被膜製造開始からの時間に対する
成膜速度の結果を第１図に示す。In the above method, the results of film formation rate versus time from the start of film production are shown in FIG.
この結果より、処理液を添加する方法にて長期にわたり
成膜速度が劣ることなく被膜の製造が行なうことが可能
であることがわかる。This result shows that it is possible to manufacture a film over a long period of time without deteriorating the film formation rate using the method of adding a treatment liquid.
［発明の効果］
本発明によれば、処理槽内の高温で過飽和状態の処理液
に対しさらに低温で略飽和状態の処理液を添加するだけ
で長時間にわたり安定した速度で被膜の形成を行うこと
ができる。[Effects of the Invention] According to the present invention, a film can be formed at a stable rate over a long period of time simply by adding a substantially saturated processing solution at a lower temperature to a processing solution that is supersaturated at a higher temperature in a processing tank. be able to.
さらにその添加量は１分あたりに処理槽内の全処理液量
の１． ２％以下であるので非常に製造コストの低い二
酸化珪素被膜を形成することができる。Furthermore, the amount added is 1.5% of the total amount of processing liquid in the processing tank per minute. Since it is 2% or less, it is possible to form a silicon dioxide film with very low manufacturing cost.
第１図は、本発明の二酸化珪素被膜製造装置を示す概略
系統図である。
第２図は、本発明による二酸化珪素被膜の製造方法にお
ける時間経過と連続成膜状況の結果を示す図である。
１・・・処理液調合槽、 ２・・・処理液保存槽３
・・・処理槽、 ４・・・冷却器５・・・ス
ターク−６・・・ヒーターFIG. 1 is a schematic system diagram showing a silicon dioxide film manufacturing apparatus of the present invention. FIG. 2 is a diagram showing the results of continuous film formation over time in the method of manufacturing a silicon dioxide film according to the present invention. 1... Processing liquid mixing tank, 2... Processing liquid storage tank 3
...Processing tank, 4...Cooler 5...Stark-6...Heater
Claims (2)
液の溶液温度を上昇させて得られる二酸化珪素の過飽和
状態の珪弗化水素酸溶液を含む処理液と基材とを接触さ
せて基材表面に二酸化珪素を析出させる二酸化珪素被膜
の製造方法において、基材を接触させた後の処理液温度
を高温に維持した状態で該処理液中に、別途低温におい
て調整した二酸化珪素が略飽和状態である珪弗化水素酸
溶液を添加することにより、該処理液中の二酸化珪素を
過飽和状態に保つことを特徴とする二酸化珪素被膜の製
造方法。(1) A substrate is brought into contact with a treatment solution containing a supersaturated hydrosilicic acid solution of silicon dioxide, which is obtained by increasing the solution temperature of a hydrosilicic acid solution in which silicon dioxide is substantially saturated. In a method for producing a silicon dioxide film in which silicon dioxide is deposited on the surface of a substrate, silicon dioxide, which has been separately adjusted at a low temperature, is added to the treatment solution while maintaining the temperature of the treatment solution at a high temperature after contacting the substrate. A method for producing a silicon dioxide film, characterized in that silicon dioxide in the treatment liquid is maintained in a supersaturated state by adding a substantially saturated hydrofluorosilicic acid solution.
液の溶液温度を上昇させて得られる二酸化珪素の過飽和
状態の珪弗化水素酸溶液を含む処理液と基材とを接触さ
せて基材表面に二酸化珪素を析出させる二酸化珪素被膜
の製造装置において、珪弗化水素酸溶液に二酸化珪素を
溶解し処理液を作製するために攪拌器（５）を有し珪弗
化水素酸溶液を恒温に保つための加熱及び／または冷却
手段を有する恒温槽内に設けられた処理液調合槽（１）
と、調合された処理液を恒温に保つため同じく恒温槽内
に設けられた処理液保存槽（２）と、基材表面に二酸化
珪素被膜を形成するために基材を浸漬する浸漬部（７）
と、浸漬部に流れ込む処理液の流れを整えるために浸漬
部に連なって設けられた整流部（９）と、浸漬部から処
理液がオーバーフローにより流れ込みさらに処理液が添
加される添加部（１０）からなり、浸漬部と整流部との
境界に設けられた整流板（８）を有し、さらに処理液温
度を所定の温度まで上昇させ恒温に保つための加熱手段
を有する処理槽（３）からなり、さらに処理槽内の処理
液を循環するための送液管（１１Ｄ）と送液管の途中に
設けられた送液ポンプ（１２Ｄ）及び処理液濾過フィル
ター（１３Ｂおよび１３Ｃ）を有し、さらに処理液調合
槽内の処理液を処理液保存槽に送液するための送液管（
１１Ａ）と送液管の途中に設けられた送液ポンプ（１２
Ａ）及び処理液濾過フィルター（１３Ａ）を有し、さら
に処理液保存槽内の処理液を処理槽整流部へ、また処理
槽浸漬部内の処理液を処理液調合槽へ送るための送液管
（それぞれ１１Ｂ、１１Ｃ）と送液管の途中にそれぞれ
設けられた送液ポンプ（それぞれ１２Ｂ、１２Ｃ）を有
する二酸化珪素被膜の製造装置。(2) The base material is brought into contact with a treatment liquid containing a supersaturated hydrosilicofluoric acid solution of silicon dioxide, which is obtained by increasing the solution temperature of a hydrosilicofluoric acid solution in which silicon dioxide is substantially saturated. A silicon dioxide film manufacturing apparatus in which silicon dioxide is deposited on the surface of a substrate using a stirrer (5) for dissolving silicon dioxide in a hydrosilicofluoric acid solution to prepare a treatment solution. Processing liquid preparation tank (1) installed in a constant temperature bath with heating and/or cooling means to keep the solution at a constant temperature
, a treatment liquid storage tank (2) which is also provided in the constant temperature bath to keep the prepared treatment liquid at a constant temperature, and a dipping section (7) in which the substrate is immersed in order to form a silicon dioxide film on the surface of the substrate. )
, a rectifying part (9) provided in series with the immersing part to regulate the flow of the processing liquid flowing into the immersing part, and an addition part (10) into which the processing liquid flows from the immersing part by overflow and further processing liquid is added. From the processing tank (3), which has a rectifying plate (8) provided at the boundary between the immersion part and the rectifying part, and further has a heating means to raise the temperature of the processing liquid to a predetermined temperature and maintain it at a constant temperature. It further has a liquid feeding pipe (11D) for circulating the processing liquid in the processing tank, a liquid feeding pump (12D) provided in the middle of the liquid feeding pipe, and processing liquid filtration filters (13B and 13C), In addition, a liquid supply pipe (
11A) and the liquid feeding pump (12
A) and a processing liquid filtration filter (13A), and a liquid sending pipe for sending the processing liquid in the processing liquid storage tank to the processing tank rectifying section and the processing liquid in the processing tank immersion section to the processing liquid mixing tank. (11B, 11C, respectively) and a liquid feeding pump (12B, 12C, respectively) provided in the middle of a liquid feeding pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1249657A JPH0798652B2 (en) | 1989-09-26 | 1989-09-26 | Method and apparatus for producing silicon dioxide film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1249657A JPH0798652B2 (en) | 1989-09-26 | 1989-09-26 | Method and apparatus for producing silicon dioxide film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03112806A true JPH03112806A (en) | 1991-05-14 |
| JPH0798652B2 JPH0798652B2 (en) | 1995-10-25 |
Family
ID=17196281
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1249657A Expired - Fee Related JPH0798652B2 (en) | 1989-09-26 | 1989-09-26 | Method and apparatus for producing silicon dioxide film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0798652B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009184913A (en) * | 2009-02-20 | 2009-08-20 | Shibaura Institute Of Technology | Recovering method of glass material |
-
1989
- 1989-09-26 JP JP1249657A patent/JPH0798652B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009184913A (en) * | 2009-02-20 | 2009-08-20 | Shibaura Institute Of Technology | Recovering method of glass material |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0798652B2 (en) | 1995-10-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH08225957A (en) | Aerosol process for manufacture of planer waveguide | |
| JP3320440B2 (en) | Coating liquid for film formation and method for producing the same | |
| US5376176A (en) | Silicon oxide film growing apparatus | |
| JPH03112806A (en) | Production of coating film of silicon dioxide and device therefor | |
| WO1992007793A1 (en) | Process for preparing silicon dioxide coating | |
| JPS6365621B2 (en) | ||
| JP3694900B2 (en) | Method for producing silica-based coating | |
| JPS6112034A (en) | Formation of silicon oxide film on silicon substrate surface | |
| JPH1036140A (en) | Liquid for treating surface of silica glass jig and treatment with the same | |
| EP0834488A1 (en) | Process for forming silica film and composition therefor | |
| JPH0538016Y2 (en) | ||
| CN113560989A (en) | Production method for processing high-precision lens by novel polishing solution | |
| JPH03285821A (en) | Production of titanium oxide coating film | |
| JPH0426528A (en) | Production of cerium oxide sol | |
| JPH02289414A (en) | Production of silicon dioxide film | |
| JPH0616427A (en) | Production of silica glass | |
| JPH1046317A (en) | Production of titanium oxide thin film | |
| JPH07165411A (en) | Production of silicon dioxide film and apparatus therefor | |
| JPH02167812A (en) | Method for producing silicon dioxide coating film | |
| JP4688115B2 (en) | Method for forming film in liquid phase | |
| JPH04310514A (en) | Production of silicon oxide-coated substrate | |
| JPH06271310A (en) | Formation of silicon dioxide film | |
| JPH07144911A (en) | Production of silicon dioxide coating film | |
| JP2953031B2 (en) | Method of forming insulating film | |
| JPH07101714A (en) | Production of silicon dioxide coating film and device therefor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |