JPS6365620B2 - - Google Patents
Info
- Publication number
- JPS6365620B2 JPS6365620B2 JP57041234A JP4123482A JPS6365620B2 JP S6365620 B2 JPS6365620 B2 JP S6365620B2 JP 57041234 A JP57041234 A JP 57041234A JP 4123482 A JP4123482 A JP 4123482A JP S6365620 B2 JPS6365620 B2 JP S6365620B2
- Authority
- JP
- Japan
- Prior art keywords
- glass
- mol
- silica
- boric acid
- treatment
- 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
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 57
- 239000011521 glass Substances 0.000 claims description 31
- 239000000377 silicon dioxide Substances 0.000 claims description 28
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 21
- 239000004327 boric acid Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 20
- 238000011282 treatment Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 11
- 229910052783 alkali metal Inorganic materials 0.000 claims description 9
- 150000001340 alkali metals Chemical class 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 4
- 239000000758 substrate Substances 0.000 description 8
- 239000004973 liquid crystal related substance Substances 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000005357 flat glass Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000011221 initial treatment Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
Landscapes
- Surface Treatment Of Glass (AREA)
- Chemically Coating (AREA)
Description
【発明の詳細な説明】
本発明はナトリウム等のアルカリ金属を含むガ
ラスの表面にシリカ膜を形成するる表面処理法に
関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a surface treatment method for forming a silica film on the surface of glass containing an alkali metal such as sodium.
一般に液晶表示パネル等のデイスプレイパネル
基板やウエハー分野でのハードマスク基板にガラ
ス基板が用いられる。これらのガラス基板には表
面が化学的に安定な石英ガラスを用いるのが好ま
しいが価格が高価となるため通常はほうけい酸ガ
ラス、ソーダライムガラス等のアルカリ金属を含
むガラスを使用することが多い。 Glass substrates are generally used for display panel substrates such as liquid crystal display panels and hard mask substrates in the wafer field. It is preferable to use quartz glass, which has a chemically stable surface, for these glass substrates, but since it is expensive, glass containing alkali metals, such as borosilicate glass or soda lime glass, is usually used. .
ナトリウム等のアルカリ金属を含むガラスは長
期の間にはその表面にアルカリ金属が析出して、
そのガラスを基板として用いた前記液晶表示パネ
ルあるいはハードマスク等の機能に悪影響を及ぼ
す。例えば、液晶表示パネルの基板にナトリウム
を含むガラスを用いるとガラス基板の表面に析出
したナトリウムが液晶中に溶出し液晶を劣化し、
ひいては液晶表示パネルの寿命を短くする。 Over a long period of time, alkali metals will precipitate on the surface of glass containing alkali metals such as sodium.
This adversely affects the functions of the liquid crystal display panel or hard mask using the glass as a substrate. For example, when glass containing sodium is used as the substrate of a liquid crystal display panel, the sodium deposited on the surface of the glass substrate dissolves into the liquid crystal and deteriorates the liquid crystal.
This in turn shortens the life of the liquid crystal display panel.
従来アルカリ金属を含むガラスの表面にアルカ
リが析出するのを防止するための真空蒸着法によ
るSiO2のコーテイングが用いられてきたが真空
蒸着法では装置が高価であるためコスト高となり
又、小さいガラスしか処理できないという欠点が
あつた。 Conventionally, coating of SiO 2 by vacuum evaporation method has been used to prevent the precipitation of alkali on the surface of glass containing alkali metals. The drawback was that it could only be processed.
本発明者らは上記従来技術の問題を解決する方
法について実験検討を重ねた結果、シリカを飽和
状態または過飽和状態に溶解した濃度が0.5ない
し3.0mol／の珪弗化水素酸水溶液にホウ酸を
１につき2.0×10-2mol以上添加した処理液を用
い、この処理液にアルカリ金属含有ガラスを浸漬
すると膜厚の一様なシリカ膜が得られることを見
い出し、この知見に基づくガラスの表面処理方法
を特願昭56−82203として提案した。 As a result of repeated experimental studies on methods for solving the problems of the prior art described above, the present inventors found that boric acid was added to an aqueous solution of hydrosilicofluoric acid with a concentration of 0.5 to 3.0 mol/in which silica was dissolved in a saturated or supersaturated state. We discovered that a silica film with a uniform thickness could be obtained by immersing alkali metal-containing glass in a treatment solution containing 2.0×10 -2 mol or more of silica. Based on this knowledge, we developed a method for surface treatment of glass. The method was proposed as a patent application 1982-82203.
上記方法によれば真空蒸着法のように真空室が
不要で大型のガラス基板に対しても非常に安価な
設備で簡単にシリカ保護膜を形成できるようにな
つたが、ガラス板の浸漬処理を繰り返し行なつて
いると処理回数を重ねるに従つてシリカ膜生成速
度が減少し、同一膜厚を形成させるにはシリカ析
出時間を長くする等の対策が必要であつた。 The above method does not require a vacuum chamber like the vacuum evaporation method, and it has become possible to easily form a silica protective film on large glass substrates using very inexpensive equipment. When the process is repeated, the rate of silica film formation decreases as the number of treatments increases, and measures such as lengthening the silica precipitation time are required to form the same film thickness.
ガラスの中からのアルカリの溶出防止には、約
1000オングストローム以上の膜厚が必要であり一
定の膜厚を形成させる必要がある。実生産工程を
考えた場合、一定時間の処理で同じ膜厚をつくる
ようにすることが好ましい。この問題点を解決す
べく種々検討を行つた結果、処理したガラスの表
面積に対応する特定量の少量のホウ酸（H3BO3）
を処理液に添加するだけで同じく析出速度と膜質
を維持できることを見出した。 To prevent alkali from leaching out of glass, approximately
A film thickness of 1000 angstroms or more is required, and it is necessary to form a film with a constant thickness. When considering the actual production process, it is preferable to create the same film thickness in a certain period of time. As a result of various studies to solve this problem, we found that a small amount of boric acid (H 3 BO 3 ) corresponding to the surface area of the treated glass was used.
It was discovered that the same deposition rate and film quality could be maintained by simply adding .
本発明は上記知見に基づいて完成したものであ
り、アルカリ金属を含むガラスを珪弗化水素酸の
シリカ飽和水溶液にホウ酸を添加した処理後に浸
漬してシリカ膜を形成させるに当り、シリカ膜形
成処理後、一定量のほう酸の添加を行なつて処理
液のシリカ膜生成能力をほぼ当初に回復させ、こ
れを繰返し行なつて常に一定膜厚、一定速度のシ
リカ膜形成が行なわれるよう制御することを要旨
としている。 The present invention was completed based on the above knowledge, and when forming a silica film by immersing glass containing an alkali metal in a silica-saturated aqueous solution of hydrosilicic acid with boric acid added, After the formation process, a certain amount of boric acid is added to restore the silica film forming ability of the processing solution to almost the initial level, and this is repeated to control the silica film formation so that it always has a constant thickness and a constant speed. The gist is to do so.
本発明を実施する場合、まず濃度が0.5ないし
3.0mol／好ましくは１〜2.5mol／のシリカ
飽和の珪弗化水素酸水溶液に1.5×10-2mol〜4.0
×10-2molの範囲内でホウ酸を添加して当初の処
理液をつくる。 When carrying out the present invention, first the concentration is 0.5 to
1.5 × 10 −2 mol to 4.0 mol/preferably 1 to 2.5 mol/silica-saturated aqueous hydrosilicic acid solution
The initial treatment solution is prepared by adding boric acid within the range of ×10 -2 mol.
この処理液中に予め定めた標準表面積量の板、
パイプ等のガラス物品を浸漬処理して所期厚み例
えば1600オングストローム厚のシリカ膜を表面に
形成した後ガラス物品を取り出す。 A plate with a predetermined standard surface area in this treatment solution,
After a glass article such as a pipe is subjected to a dipping treatment to form a silica film having a desired thickness, for example, 1600 angstroms, on the surface, the glass article is taken out.
次にこの処理液に試験用の上記と同一組成のガ
ラスを浸漬し、ホウ酸の添加量を少しづつ例えば
１×10-3mol単位で変えてそれぞれの添加量にお
ける生成シリカ膜厚を測定し、両者の関係を求め
ておく。 Next, a test glass with the same composition as above was immersed in this treatment solution, and the amount of boric acid added was changed little by little, for example, in units of 1 x 10 -3 mol, and the thickness of the silica film formed at each addition amount was measured. , find the relationship between the two.
ホウ酸の添加量は１×10-3mol／以下ではシ
リカの析出速度が低下して膜ができない。又一方
６×10-3mol／以上になると析出速度が増加し
て液中に沈澱を生ずる。従つて１×10-3〜６×
10-3mol／が好ましい。 If the amount of boric acid added is less than 1 x 10 -3 mol/, the rate of silica precipitation decreases and a film cannot be formed. On the other hand, when the amount exceeds 6×10 -3 mol/, the precipitation rate increases and precipitation occurs in the liquid. Therefore, 1×10 -3 ~6×
10 -3 mol/ is preferred.
そして上記生成シリカ膜厚が前述した所期厚
み、例えば1600オングストロームの膜厚に対応す
るホウ酸添加量を以後の標準総面積のガラス１回
処理毎の添加量とする。 Then, the amount of boric acid added corresponding to the above-mentioned desired thickness of the generated silica film, for example, 1600 angstroms, is set as the amount of boric acid added for each subsequent glass treatment of the standard total area.
また処理するガラスの全表面積が上記標準表面
積と相違する場合は両者の表面積比を上記標準添
加量に掛ければホウ酸の必要添加量を求めること
ができる。 If the total surface area of the glass to be treated differs from the above standard surface area, the required addition amount of boric acid can be determined by multiplying the above standard addition amount by the ratio of both surface areas.
本発明処理方法におけるシリカ膜生成機構につ
いては充分に解明はされていないが、珪弗化水素
酸（H2SiF6）にホウ酸を添加することにより
H2SiF6がSiO2とHBF4とに分解促進され、その
結果SiO2が浸漬ガラス表面に析出されると考え
られる。 The mechanism of silica film formation in the treatment method of the present invention has not been fully elucidated, but by adding boric acid to hydrosilicofluoric acid (H 2 SiF 6 ),
It is thought that H 2 SiF 6 is promoted to decompose into SiO 2 and HBF 4 , and as a result, SiO 2 is deposited on the surface of the immersed glass.
なお本発明は処理するガラスの組成を特に制限
するものではない。 Note that the present invention does not particularly limit the composition of the glass to be treated.
以下に実施例を述べる。 Examples will be described below.
実施例 １
組成がSiO2：78.2重量％、Al2O3：1.76重量％、
MgO：4.03重量％、CaO：7.27重量％、Na2O：
13.1重量％、K2O：0.79重量％である板ガラスを
表面の汚れを除去するために、0.5％HFに10分間
浸漬し、水洗後処理液１に対して2.5×10-2mol
のホウ酸を添加した1.5mol／のシリカ飽和珪
弗化水素酸水溶液に35℃で24時間浸漬したところ
約1600オングストローム厚みのシリカ膜が表面に
生成した。この処理液に１×10-3mol／から６
×10-3mol／まで１×10-3mol／きざみでホ
ウ酸を0.5mol／の水溶液の形で添加した処理
液をそれぞれ用意し、この液に上記と同一組成で
同一の大きさの試験用板ガラスを24時間浸漬した
ところホウ酸を２×10-3mol／添加した処理液
については約1600オングストロームのシリカ膜が
生成し、これより少ないものは薄く多いものは厚
くなることがわかつたので引続き２×10-3mol／
を添加した処理液を用いてシリカ膜生成を行な
い、同様の工程を繰り返して約1600オングストロ
ーム厚みのシリカ膜を設けた多数のガラス板を毎
回ほぼ同一の膜厚と処理時間で製造することがで
きた。Example 1 Composition: SiO 2 : 78.2% by weight, Al 2 O 3 : 1.76% by weight,
MgO: 4.03 wt%, CaO: 7.27 wt%, Na2O :
In order to remove surface stains, a plate glass containing 13.1% by weight and 0.79% by weight of K 2 O was immersed in 0.5% HF for 10 minutes, and 2.5×10 -2 mol per 1 part of the treatment solution after washing with water was immersed in 0.5% HF for 10 minutes.
When the sample was immersed for 24 hours at 35°C in a 1.5 mol silica-saturated aqueous solution of hydrofluorosilicic acid to which boric acid had been added, a silica film about 1600 angstroms thick was formed on the surface. This treatment solution contains 1×10 -3 mol/ to 6
Prepare a treatment solution in which boric acid is added in the form of a 0.5 mol/aqueous solution in steps of 1 x 10 -3 mol/up to ×10 -3 mol/, and add a test solution of the same composition and size as above to this solution. When a glass plate was immersed for 24 hours, a silica film of approximately 1600 angstroms was formed in a treatment solution containing 2 x 10 -3 mol of boric acid, and it was found that those with less than this were thinner and those with more than this were thicker. Continued to be 2×10 -3 mol/
A silica film is produced using a processing solution containing 1,600 angstroms of silica, and by repeating the same process, it is possible to produce a large number of glass plates with approximately 1,600 angstrom thick silica films each time using approximately the same film thickness and processing time. Ta.
実施例 ２
組成がSiO2：73.2重量％、Al2O3：1.90重量％、
MgO：0.12重量％、CaO：8.67重量％、Na2O：
14.3重量％、K2O：0.06重量％である板ガラスを
表面の汚れを除去するために0.5％HFに10分間浸
漬し水洗後、処理液１に対し、2.8×10-2molの
のホウ酸を添加した濃度1.5mol／のシリカ飽
和珪弗化水素酸水溶液に35℃で20時間浸漬したと
ころガラス表面に約2400オングストロームのシリ
カ膜が生成した。この処理液に実施例１と同様に
１×10-3mol／から６×10-3mol／の範囲で、
ホウ酸を添加した液をそれぞれ用意し、これら液
に上記と同称の前処理を行つた板ガラスをそれぞ
れ20時間浸漬したところ３×10-3mol／添加し
た処理液については約2400オングストロームのシ
リカ膜が生成しこれよりホウ酸添加量が少ないも
のはシリカ膜厚みが薄く多いものはより厚膜とな
つた。Example 2 Composition: SiO 2 : 73.2% by weight, Al 2 O 3 : 1.90% by weight,
MgO: 0.12 wt%, CaO: 8.67 wt%, Na2O :
A plate glass containing 14.3% by weight and 0.06% by weight of K 2 O was immersed in 0.5% HF for 10 minutes to remove surface stains, and after washing with water, 2.8 x 10 -2 mol of boric acid was added to 1 of the treatment solution. When the glass was immersed for 20 hours at 35°C in an aqueous solution of silica-saturated hydrofluorosilicic acid at a concentration of 1.5 mol/ml, a silica film of approximately 2400 angstroms was formed on the glass surface. In this treatment solution, as in Example 1, in the range of 1 × 10 -3 mol/ to 6 × 10 -3 mol/,
We prepared solutions to which boric acid had been added, and immersed plate glasses that had been pretreated in the same manner as above for 20 hours in these solutions, resulting in approximately 2,400 angstroms of silica for the solution containing 3 x 10 -3 mol of boric acid. A film was formed, and when the amount of boric acid added was less, the silica film was thinner, and when it was added, the silica film was thicker.
以後引続き３×10-3mol／を添加した処理液
に１回のガラス板処理を終える毎に同一量のホウ
酸を加え繰返し約2400オングストローム厚で一定
のシリカ膜をほぼ同じ処理時間で生成した。 Thereafter, the same amount of boric acid was added to the treatment solution containing 3 x 10 -3 mol/each time each glass plate treatment was completed, and a silica film with a constant thickness of approximately 2400 angstroms was produced in approximately the same treatment time. .
Claims (1)
3.0mol／の珪弗化水素酸のシリカ飽和水溶液
に1.5×10-2〜4.0×10-2mol／のホウ酸を添加
した処理液に浸漬することにより、該ガラス表面
上にシリカ膜を形成させる表面処理方法におい
て、ガラスの浸漬処理後に、処理液に１×10-3〜
６×10-3mol／のホウ酸を添加して処理液のシ
リカ膜生成能力を一定に維持しつつ繰返し使用す
ることを特徴とするアルカリ金属を含むガラスの
表面処理法。1 Glass containing alkali metals at a concentration of 0.5~
A silica film is formed on the glass surface by immersing it in a treatment solution in which 1.5 × 10 -2 - 4.0 × 10 -2 mol / boric acid is added to a 3.0 mol / silica saturated aqueous solution of hydrofluorosilicic acid. In the surface treatment method, after the glass is immersed, a concentration of 1×10 -3 ~
A method for surface treatment of glass containing an alkali metal, characterized by adding 6×10 -3 mol/boric acid and repeatedly using the treatment solution while maintaining a constant silica film forming ability.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4123482A JPS58161944A (en) | 1982-03-16 | 1982-03-16 | Surface treatment of glass containing alkali metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4123482A JPS58161944A (en) | 1982-03-16 | 1982-03-16 | Surface treatment of glass containing alkali metal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58161944A JPS58161944A (en) | 1983-09-26 |
| JPS6365620B2 true JPS6365620B2 (en) | 1988-12-16 |
Family
ID=12602719
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4123482A Granted JPS58161944A (en) | 1982-03-16 | 1982-03-16 | Surface treatment of glass containing alkali metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58161944A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0288924U (en) * | 1988-12-28 | 1990-07-13 | ||
| CN103695875A (en) * | 2013-12-06 | 2014-04-02 | 湖洲三峰能源科技有限公司 | Chemical composition for accelerating growth of silicon oxide on surface of substrate |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6436770A (en) * | 1987-07-30 | 1989-02-07 | Nippon Sheet Glass Co Ltd | Production of silicon dioxide film containing phosphorus |
| JP4734517B2 (en) * | 2004-04-02 | 2011-07-27 | 新コスモス電機株式会社 | Manufacturing method of gas sensor |
| WO2009096218A1 (en) * | 2008-01-30 | 2009-08-06 | Konica Minolta Opto, Inc. | Substrate manufacturing method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB626810A (en) * | 1946-08-16 | 1949-07-21 | Rca Corp | Process of depositing silica films |
| US2490662A (en) * | 1946-09-21 | 1949-12-06 | Rca Corp | Skeletonizing glass |
-
1982
- 1982-03-16 JP JP4123482A patent/JPS58161944A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB626810A (en) * | 1946-08-16 | 1949-07-21 | Rca Corp | Process of depositing silica films |
| US2490662A (en) * | 1946-09-21 | 1949-12-06 | Rca Corp | Skeletonizing glass |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0288924U (en) * | 1988-12-28 | 1990-07-13 | ||
| CN103695875A (en) * | 2013-12-06 | 2014-04-02 | 湖洲三峰能源科技有限公司 | Chemical composition for accelerating growth of silicon oxide on surface of substrate |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58161944A (en) | 1983-09-26 |
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