JPH0567709B2 - - Google Patents
Info
- Publication number
- JPH0567709B2 JPH0567709B2 JP62190620A JP19062087A JPH0567709B2 JP H0567709 B2 JPH0567709 B2 JP H0567709B2 JP 62190620 A JP62190620 A JP 62190620A JP 19062087 A JP19062087 A JP 19062087A JP H0567709 B2 JPH0567709 B2 JP H0567709B2
- Authority
- JP
- Japan
- Prior art keywords
- silicon dioxide
- dioxide film
- substrate
- treatment liquid
- concentration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 109
- 239000000377 silicon dioxide Substances 0.000 claims description 53
- 235000012239 silicon dioxide Nutrition 0.000 claims description 53
- 239000000758 substrate Substances 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 238000000034 method Methods 0.000 description 17
- 239000000463 material Substances 0.000 description 11
- 239000002585 base Substances 0.000 description 9
- 239000005361 soda-lime glass Substances 0.000 description 8
- 239000011521 glass Substances 0.000 description 7
- 238000007654 immersion Methods 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000010828 elution Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910018626 Al(OH) Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001004 secondary ion mass spectrometry Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明はＰを含む二酸化珪素被膜の製造方法に
関し、特にアルカリ金属拡散防止膜等に有用な、
Ｐを含む二酸化珪素被膜の製造方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing a silicon dioxide film containing P, which is particularly useful as an alkali metal diffusion prevention film, etc.
The present invention relates to a method for producing a silicon dioxide film containing P.
［従来の技術］
今日、いろいろな材料の表面を二酸化珪素膜で
被覆することが広く行なわれている。例えば液晶
表示パネル、太陽電池用基板ガラスにソーダライ
ムガラスまたはホウ珪酸ガラスなどアルカリ含有
ガラスを用いる場合、ガラスからのアルカリ成分
の溶出を防止する目的で、これらのガラス表面を
二酸化珪素膜で被覆することが行なわれている。
この場合、純粋な二酸化珪素膜で被覆するよりも
Ｐを含む二酸化珪素膜で被覆したほうがガラスか
らのアルカリ成分の溶出を防止する能力が高いこ
とが知られている。[Prior Art] Today, it is widely practiced to coat the surfaces of various materials with silicon dioxide films. For example, when alkali-containing glasses such as soda lime glass or borosilicate glass are used for substrate glass for liquid crystal display panels and solar cells, the surfaces of these glasses are coated with a silicon dioxide film in order to prevent the elution of alkaline components from the glass. things are being done.
In this case, it is known that coating with a silicon dioxide film containing P has a higher ability to prevent elution of alkaline components from the glass than coating with a pure silicon dioxide film.
基材の表面にＰを含む二酸化珪素被膜を形成さ
せるには、CVD法や塗布法等の方法が多く用い
られてきた。たとえばCVD法では(1)式の反応に
よりＰを含む二酸化珪素被膜を形成させ
SiH4＋2PH3＋6O2→SiO2＋P2O5＋5H2O
(1)
ることができる。さらには、CVD法やスパツタ、
真空蒸着などの方法でいつたん二酸化珪素被膜を
形成し、イオン注入によりイオン化したＰをその
二酸化珪素被膜に打ち込むことによりＰを含む二
酸化珪素被膜を形成することも可能である。しか
し、これらの方法では、凹凸形状を有する基材表
面に均一なＰを含む二酸化珪素被膜を形成するこ
とは困難である。また、これらの方法は装置ある
いは付帯設備が高価であるため、Ｐを含む二酸化
珪素被覆に要するコストが高くなる他、小さな基
材しか処理できないという欠点があつた。 Many methods such as CVD method and coating method have been used to form a silicon dioxide film containing P on the surface of a base material. For example, in the CVD method, a silicon dioxide film containing P is formed by the reaction of formula (1) SiH 4 +2PH 3 +6O 2 →SiO 2 +P 2 O 5 +5H 2 O
(1) Can. Furthermore, CVD method, spats,
It is also possible to form a silicon dioxide film containing P by simply forming a silicon dioxide film using a method such as vacuum evaporation, and then implanting ionized P into the silicon dioxide film by ion implantation. However, with these methods, it is difficult to form a uniform P-containing silicon dioxide film on the surface of a base material having an uneven shape. In addition, these methods require expensive equipment or ancillary equipment, which increases the cost required for coating silicon dioxide containing P, and they also have the disadvantage that only small substrates can be treated.
上記Ｐを含む二酸化珪素被膜形成方法に対し、
凹凸形状を有する基材表面に均一な二酸化珪素被
膜を形成する方法として珪弗化水素酸の二酸化珪
素過飽和水溶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60−33233）
上記析出法によれば装置が簡便であり、かつ大き
な基材への二酸化珪素被覆が容易に行なえる。 For the above method for forming a silicon dioxide film containing P,
A method for forming a uniform silicon dioxide film on the surface of a substrate having an uneven shape is to immerse the substrate in a supersaturated silicon dioxide aqueous solution of hydrosilicofluoric acid to deposit a silicon dioxide film on the surface of the substrate (hereinafter referred to as the precipitation method). ) is known. (For example, JP-A-60-33233)
According to the above precipitation method, the apparatus is simple and large substrates can be easily coated with silicon dioxide.
［発明が解決しようとする問題点］
本発明は、従来法における凹凸形状を有する基
材表面に均一なＰを含む二酸化珪素被膜を形成す
ることが困難であるという問題点を解決し、さら
に大面積の基材にＰを含む二酸化珪素被膜を低コ
ストで形成させることのできるＰを含む二酸化珪
素被膜の製造方法を提供するものである。[Problems to be Solved by the Invention] The present invention solves the problem that it is difficult to form a uniform P-containing silicon dioxide film on the surface of a base material having an uneven shape in the conventional method. The present invention provides a method for producing a P-containing silicon dioxide film, which can form a P-containing silicon dioxide film on a large substrate at low cost.
［問題点を解決するための手段］
本発明は上記問題点を解決するためになされた
ものであつて、二酸化珪素の過飽和状態となつた
珪弗化水素酸水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被膜を析出させる二
酸化珪素被膜の製造方法において、該処理液中に
Ｐを含ませておくことによつて、Ｐを含む二酸化
珪素被膜を基材表面に析出形成させている。処理
液中に含ませるＰの原料としては、ＰおよびＰ化
合物等任意の原料が使用できる。[Means for Solving the Problems] The present invention has been made to solve the above-mentioned problems. In the method for producing a silicon dioxide film in which a silicon dioxide film is precipitated on the surface of a substrate by contacting with P, a silicon dioxide film containing P is precipitated on the surface of the substrate by including P in the treatment liquid. It is being formed. As the raw material for P to be included in the treatment liquid, any raw material such as P and P compounds can be used.
処理液中のＰの濃度は、濃ければ濃いほど二酸
化珪素被膜中に含まれるＰの濃度が濃くなるので
好ましいが、0.01〜5.5モル／リツトルの濃度で
使用されることが好ましい。該濃度が0.01モル／
リツトルより少ないと二酸化珪素被膜中に含まれ
るＰ濃度が低くなり本発明の効果が表われにく
い。又5.5モル／リツトルよりも高くなると、処
理液中に溶解できなくなつたり、析出のスピード
が低下したりしやすくなる。 The concentration of P in the treatment solution is preferably 0.01 to 5.5 mol/liter, since the higher the concentration of P contained in the silicon dioxide coating, the higher the concentration of P contained in the silicon dioxide coating. The concentration is 0.01 mol/
If the amount is less than a little, the P concentration contained in the silicon dioxide film will be low and the effects of the present invention will be difficult to manifest. Further, if the amount is higher than 5.5 mol/liter, it becomes difficult to dissolve in the processing solution or the speed of precipitation tends to decrease.
本発明において、該処理液の珪弗化水素酸濃度
は0.1モル／リツトル〜2.0モル／リツトルである
ことが好ましい。すなわち該処理液の珪弗化水素
酸濃度が2.0モル／リツトル以上では形成された
二酸化珪素中のＰ濃度が低く、また0.1モル／リ
ツトル以下では二酸化珪素膜が全く形成されない
か又は均一な二酸化珪素膜が形成できない。又、
該処理液と基材とを接触させている時の該処理液
の温度が０℃〜35℃であることが好ましい。すな
わち、該処理液温度が35℃以上では形成された二
酸化珪素膜中のＰ濃度が低く、また０℃以下では
処理液中の水の凍結又はH2SiF6、nH2Oの析出等
がおこる等処理液自体の安定性が悪くなる。 In the present invention, the concentration of hydrosilicofluoric acid in the treatment liquid is preferably 0.1 mol/liter to 2.0 mol/liter. That is, if the hydrosilicofluoric acid concentration of the treatment solution is 2.0 mol/liter or more, the P concentration in the formed silicon dioxide is low, and if it is 0.1 mol/liter or less, no silicon dioxide film is formed or a uniform silicon dioxide film is formed. A film cannot be formed. or,
It is preferable that the temperature of the treatment liquid during contact between the treatment liquid and the substrate is 0°C to 35°C. That is, when the temperature of the processing solution is 35°C or higher, the P concentration in the formed silicon dioxide film is low, and when it is below 0°C, freezing of water in the processing solution or precipitation of H 2 SiF 6 and nH 2 O occurs. The stability of the processing solution itself deteriorates.
上記処理液中の二酸化珪素の過飽和状態となつ
た珪弗化水素酸溶液の調整方法は特に限定され
ず、たとえばH3BO3、Al、Al（OH）3等を処理液
に添加する方法や処理液の温度を上昇させる方法
など従来知られた種々の方法が使用できる。 The method for preparing the hydrosilicofluoric acid solution in which the silicon dioxide in the treatment liquid is supersaturated is not particularly limited, and may include, for example, a method of adding H 3 BO 3 , Al, Al(OH) 3 , etc. to the treatment liquid; Various conventionally known methods can be used, such as a method of increasing the temperature of the processing liquid.
また、該処理液と基材とを接触させる方法とし
ては、該基材表面に処理液を流下させる等の接触
方法であつてもかまわないが、処理液を満たした
浸漬槽に該基材を浸漬する方法が簡単でしかも均
一な被膜が得られるので好ましい。 In addition, the method of bringing the treatment liquid into contact with the substrate may be a contact method such as flowing the treatment liquid down onto the surface of the substrate, but the substrate may be placed in an immersion tank filled with the treatment liquid. The immersion method is preferred because it is simple and provides a uniform coating.
本発明に適用される基材は、アルカリを含んだ
ガラスに限定されず、シリカガラス、無アルカリ
ガラス、各種セラミツクスやシリコン等の半導体
基板等上記析出法により二酸化珪素被膜が形成可
能であるあらゆる基材にも適用できる。またその
用途は基材からのアルカリ溶出防止だけでなく、
たとえばシリコン基材へＰを拡散するための拡散
源等として用いることも可能である。 The base material applied to the present invention is not limited to glass containing alkali, but any base material on which a silicon dioxide film can be formed by the above precipitation method, such as silica glass, alkali-free glass, various ceramics, and semiconductor substrates such as silicon. It can also be applied to materials. In addition, its uses include not only preventing alkali elution from base materials, but also
For example, it can also be used as a diffusion source for diffusing P into a silicon base material.
さらに本発明はＰのみを含む二酸化珪素被膜を
形成するためだけでなく、他の有効な１種類以上
を物質（たとえばＢを含む二酸化珪素膜はＰを含
む二酸化珪素膜と同様基材からのアルカリ溶出防
止能力が高いといわれている）と組み合わせてＰ
と他の有効な１種類以上の物質を含む二酸化珪素
被膜を形成する事にも適用できる。 Furthermore, the present invention is not only for forming a silicon dioxide film containing only P, but also for forming one or more other effective substances (for example, a silicon dioxide film containing B is similar to a silicon dioxide film containing P, and a silicon dioxide film containing P is also used to form a silicon dioxide film containing P). P is said to have high elution prevention ability).
It can also be applied to forming a silicon dioxide film containing one or more other effective substances.
［作用］
本発明によれば、均一な溶液内でＰを含む二酸
化珪素被膜を形成させるため凹凸形状を有する基
材表面にも均一な膜を得ることができる。また室
温付近の温度での成膜が可能であるため、耐熱性
の悪い基材（たとえばプラスチツク成形体）や熱
による変質がおこりやすい基材（たとえば不純物
を拡散させたシリコン）にも適用が可能である。
さらに成膜条件を変更することによりＰの含有量
を任意に調節できる。すなわち、処理液中のＰ
の濃度の増加。処理液の珪弗化水素酸濃度の低
下。処理液と基材とを接触させている時の処理
液温度の低下。等の条件を単独又は組合せて用い
ることにより該二酸化珪素被膜中のＰ濃度を増加
させることも可能である。[Function] According to the present invention, since a silicon dioxide film containing P is formed in a uniform solution, a uniform film can be obtained even on the surface of a substrate having an uneven shape. In addition, since it is possible to form a film at a temperature close to room temperature, it can be applied to substrates with poor heat resistance (for example, plastic molded bodies) or substrates that are susceptible to deterioration due to heat (for example, silicon with diffused impurities). It is.
Furthermore, the content of P can be arbitrarily adjusted by changing the film forming conditions. That is, P in the processing solution
An increase in the concentration of. Decrease in the concentration of hydrosilicofluoric acid in the treatment solution. Decrease in the temperature of the treatment liquid when the treatment liquid is in contact with the substrate. It is also possible to increase the P concentration in the silicon dioxide film by using these conditions alone or in combination.
［実施例］
平板表面上に深さ0.07μｍ、幅0.8μｍ、ピツチ
1.6μｍの溝を有するたて100mm、よこ100mm、厚さ
１mmのソーダライムガラスと表面に凹凸形状を有
しないたて100mm、よこ100mm、厚さ１mmのソーダ
ライムガラスを第１図に示す浸漬槽を用い以下の
手順で処理した。浸漬槽は外槽１と内槽２から成
り、内槽と外槽の間には水３が満してある。実験
では、この水の温度が10℃となるよう、水は温度
調節器４で調節され、かつ温度分布均一化のため
攪拌器５で攪拌されている。内槽は前部６、中部
７、後部８から成り、各部には工業用シリカゲル
粉末を溶解飽和し、かつＰ化合物としてP2O5を
0.1モル／リツトルとなるように溶解させた1.0モ
ル／リツトルの濃度の珪弗化水素酸水溶液３１が
反応液として満してある。ここでまず循環ポンプ
１０を作動させ内槽後部８の反応液を一定量ずつ
汲出してフイルター１１で濾過し内槽前部６へ戻
す処理液循環を開始した。[Example] A pitch of 0.07 μm in depth and 0.8 μm in width on the surface of a flat plate.
A soda lime glass measuring 100 mm long, 100 mm wide and 1 mm thick with a groove of 1.6 μm and a soda lime glass measuring 100 mm long, 100 mm wide and 1 mm thick with no uneven surface on the immersion tank shown in Figure 1. was processed using the following procedure. The immersion tank consists of an outer tank 1 and an inner tank 2, and water 3 is filled between the inner tank and the outer tank. In the experiment, the water was regulated with a temperature controller 4 so that the temperature of the water was 10° C., and was stirred with a stirrer 5 to make the temperature distribution uniform. The inner tank consists of a front part 6, a middle part 7, and a rear part 8, and each part is saturated with industrial silica gel powder and contains P 2 O 5 as a P compound.
An aqueous solution of hydrosilicic acid fluoride 31 having a concentration of 1.0 mol/liter is filled as a reaction liquid. First, the circulation pump 10 was operated to pump out a certain amount of the reaction liquid from the rear part 8 of the inner tank, filter it with the filter 11, and start circulating the treated liquid back to the front part 6 of the inner tank.
その後0.5モル／リツトルのホウ酸水溶液１２
を連続的に内槽後部８に滴下し、10時間保持し
た。この状態で反応液は適度なSiO2過飽和度を
有する処理液となつた。ここでフイルター１１の
絶対除去率を1.5μｍおよび処理液循環流量を240
ml／min（距離液全量が約３リツトルであるので
循環量は約８％／minである）と調整した。そし
て前記ソーダライムガラス９を内槽中部７に垂直
に浸漬し、前記条件（0.5モル／リツトルのホウ
酸水溶液を0.2ml／minで添加し、８％／minの循
環をし、1.5μｍのフイルターで濾過する）で４時
間保持した。 Then 0.5 mol/liter boric acid aqueous solution 12
was continuously dropped into the rear part 8 of the inner tank and maintained for 10 hours. In this state, the reaction solution became a treatment solution with an appropriate degree of SiO 2 supersaturation. Here, the absolute removal rate of filter 11 is 1.5 μm and the processing liquid circulation flow rate is 240 μm.
ml/min (since the total amount of liquid is about 3 liters, the circulation rate is about 8%/min). Then, the soda lime glass 9 was immersed vertically into the inner tank middle part 7, and under the conditions described above (0.5 mol/liter boric acid aqueous solution was added at 0.2 ml/min, circulated at 8%/min, and passed through a 1.5 μm filter. The mixture was filtered for 4 hours.
上記処理で得られた二酸化珪素被膜の膜厚は平
板のソーダライムガラスで約120nｍであつた。
上記平板のソーダライムガラム上に形成された二
酸化珪素被膜について二次イオン質量分析により
表面から深さ方向へ組成分析を行なつた。その結
果二酸化珪素膜中ではSi、Ｏの他Ｐが検出され、
Ｐの濃度は約0.03重量％であることがわかつた。
一方、上記表面に凹凸を有するソーダライムガラ
ス上に形成された二酸化珪素被膜についてその破
断面のSEM観察を行なつた。その結果、二酸化
珪素被膜は基板であるソーダライムガラスの形状
に追従して形成されており、かつその膜厚は凸
部、凹部ともにほとんど差がみられなかつた。 The thickness of the silicon dioxide film obtained by the above treatment was about 120 nm on a flat soda lime glass plate.
The composition of the silicon dioxide film formed on the above-mentioned flat soda lime garum was analyzed from the surface to the depth direction by secondary ion mass spectrometry. As a result, Si, O, and P were detected in the silicon dioxide film.
The concentration of P was found to be approximately 0.03% by weight.
On the other hand, SEM observation of the fractured surface of the silicon dioxide coating formed on the soda lime glass having the uneven surface was performed. As a result, the silicon dioxide film was formed to follow the shape of the soda lime glass substrate, and there was almost no difference in the film thickness between the convex and concave portions.
［発明の効果］
本発明によれば、実施例でも明らかなように、
凹凸形状を有する基材表面にも均一なＰを含む二
酸化珪素被膜を低コストで形成することができ
る。さらに大面積の基材への適用も容易である。[Effects of the Invention] According to the present invention, as is clear from the examples,
A uniform silicon dioxide film containing P can be formed at low cost even on the surface of a base material having an uneven shape. Furthermore, it is easy to apply to large-area base materials.
第１図は実施例において使用した浸漬槽の系統
説明図である。
１……外槽、２……内槽、３……水、４……温
度調節器、５……攪拌器、６……内槽前部、７…
…内槽中央部、８……内槽後部、９……ソーダラ
イムガラス、１０……循環ポンプ、１１……フイ
ルター、１２……ホウ酸水溶液。
FIG. 1 is a system explanatory diagram of the immersion tank used in the example. 1... Outer tank, 2... Inner tank, 3... Water, 4... Temperature controller, 5... Stirrer, 6... Inner tank front, 7...
...Inner tank center, 8...Inner tank rear, 9...Soda lime glass, 10...Circulation pump, 11...Filter, 12...Boric acid aqueous solution.
Claims (1)
酸水溶液を含む処理液と基材とを接触させて基材
表面に二酸化珪素被膜を析出させる二酸化珪素被
膜の製造方法において、該処理液中に0.01〜5.5
モル／リツトルの濃度のＰを含ませておくことに
より、Ｐを含む二酸化珪素被膜を基材表面に析出
形成させることを特徴とするＰを含む二酸化珪素
被膜の製造方法。 ２ 該処理液の珪弗化水素酸濃度が0.1〜2.0モ
ル／リツトルである特許請求の範囲第１項に記載
のＰを含む二酸化珪素被膜の製造方法。 ３ 該処理液と基材を接触させている時の該処理
液の温度が０℃〜35℃である特許請求の範囲第１
項または第２項記載のＰを含む二酸化珪素被膜の
製造方法。[Scope of Claims] 1. A method for producing a silicon dioxide coating, in which a silicon dioxide coating is deposited on the surface of a substrate by bringing the substrate into contact with a treatment solution containing an aqueous solution of hydrosilicic acid in which silicon dioxide is supersaturated. , 0.01 to 5.5 in the processing solution
A method for producing a P-containing silicon dioxide film, which comprises precipitating and forming a P-containing silicon dioxide film on the surface of a substrate by incorporating P at a concentration of mole/liter. 2. The method for producing a P-containing silicon dioxide film according to claim 1, wherein the treatment liquid has a hydrosilicofluoric acid concentration of 0.1 to 2.0 mol/liter. 3. Claim 1, wherein the temperature of the treatment liquid when the treatment liquid is in contact with the substrate is 0°C to 35°C.
A method for producing a silicon dioxide film containing P according to item 1 or 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19062087A JPS6436770A (en) | 1987-07-30 | 1987-07-30 | Production of silicon dioxide film containing phosphorus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19062087A JPS6436770A (en) | 1987-07-30 | 1987-07-30 | Production of silicon dioxide film containing phosphorus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6436770A JPS6436770A (en) | 1989-02-07 |
| JPH0567709B2 true JPH0567709B2 (en) | 1993-09-27 |
Family
ID=16261101
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19062087A Granted JPS6436770A (en) | 1987-07-30 | 1987-07-30 | Production of silicon dioxide film containing phosphorus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6436770A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5903848B2 (en) * | 2011-11-25 | 2016-04-13 | 三菱マテリアル株式会社 | Glass substrate with antireflection film |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57196744A (en) * | 1981-05-29 | 1982-12-02 | Nippon Sheet Glass Co Ltd | Surface treatment of glass containing alkali metal |
| JPS58161944A (en) * | 1982-03-16 | 1983-09-26 | Nippon Sheet Glass Co Ltd | Surface treatment of glass containing alkali metal |
| JPS6033233A (en) * | 1983-07-27 | 1985-02-20 | Nippon Sheet Glass Co Ltd | Preparation of glass coated with silicon oxide |
| JPS6048740A (en) * | 1983-08-29 | 1985-03-16 | 高橋 孝輔 | Erection aid tool of penis |
| JPS62158136A (en) * | 1985-12-27 | 1987-07-14 | Nippon Soda Co Ltd | Glass substrate |
-
1987
- 1987-07-30 JP JP19062087A patent/JPS6436770A/en active Granted
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57196744A (en) * | 1981-05-29 | 1982-12-02 | Nippon Sheet Glass Co Ltd | Surface treatment of glass containing alkali metal |
| JPS58161944A (en) * | 1982-03-16 | 1983-09-26 | Nippon Sheet Glass Co Ltd | Surface treatment of glass containing alkali metal |
| JPS6033233A (en) * | 1983-07-27 | 1985-02-20 | Nippon Sheet Glass Co Ltd | Preparation of glass coated with silicon oxide |
| JPS6048740A (en) * | 1983-08-29 | 1985-03-16 | 高橋 孝輔 | Erection aid tool of penis |
| JPS62158136A (en) * | 1985-12-27 | 1987-07-14 | Nippon Soda Co Ltd | Glass substrate |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6436770A (en) | 1989-02-07 |
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