JP2725211B2 - Glass surface treatment method - Google Patents
Glass surface treatment methodInfo
- Publication number
- JP2725211B2 JP2725211B2 JP1258224A JP25822489A JP2725211B2 JP 2725211 B2 JP2725211 B2 JP 2725211B2 JP 1258224 A JP1258224 A JP 1258224A JP 25822489 A JP25822489 A JP 25822489A JP 2725211 B2 JP2725211 B2 JP 2725211B2
- Authority
- JP
- Japan
- Prior art keywords
- acid solution
- glass
- treatment method
- glass surface
- surface 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 - Fee Related
Links
- 239000011521 glass Substances 0.000 title claims description 22
- 238000000034 method Methods 0.000 title claims description 22
- 238000004381 surface treatment Methods 0.000 title claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- 239000002253 acid Substances 0.000 claims description 14
- 239000005355 lead glass Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 10
- 239000010410 layer Substances 0.000 description 10
- 229910017604 nitric acid Inorganic materials 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000010306 acid treatment Methods 0.000 description 7
- 238000011282 treatment Methods 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 239000005357 flat glass Substances 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011369 optimal treatment Methods 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は重量％でPbOを50％以上含有する高鉛ガラス
の表面に反射防止層を形成するためのガラス表面処理方
法に関するものである。Description: TECHNICAL FIELD The present invention relates to a glass surface treatment method for forming an antireflection layer on the surface of high lead glass containing 50% by weight or more of PbO by weight.
従来より、窓ガラス及び板ガラス等のガラス表面に反
射防止処理を施す方法として真空蒸着法、コーティング
法、酸処理法等が知られている。BACKGROUND ART Conventionally, a vacuum deposition method, a coating method, an acid treatment method, and the like have been known as methods for performing antireflection treatment on a glass surface such as a window glass and a plate glass.
しかしながら真空蒸着法は、その装置の制約から処理
するガラスの大きさに限界があり、それゆえ大型で厚み
のあるガラスの処理には不向きである。またコーティン
グ法では、被覆する反射防止膜が単層であれば、狭い波
長帯でしか低い全反射率を得ることができない。したが
ってこの方法において、比較的広い波長帯にわたって低
い全反射率を得るためには反射防止膜を多層構造にする
必要があり、作業が複雑になり手間がかかる。さらにこ
れら二つの方法はコストが高くなるという欠点を有す
る。このため放射線の遮蔽に用いるような鉛ガラスに反
射防止処理を施す場合には、酸処理法による処理が一般
的である。However, the vacuum deposition method has a limitation in the size of the glass to be processed due to the limitation of the apparatus, and therefore is not suitable for processing a large and thick glass. In the coating method, a low total reflectance can be obtained only in a narrow wavelength band if the covering antireflection film is a single layer. Therefore, in this method, in order to obtain a low total reflectance over a relatively wide wavelength band, the antireflection film needs to have a multilayer structure, which makes the operation complicated and time-consuming. Furthermore, these two methods have the disadvantage of high costs. For this reason, when antireflection treatment is performed on lead glass used for shielding radiation, an acid treatment method is generally used.
酸処理法による反射防止処理には通常硝酸溶液を酸と
して用いるが、これはガラスを酸処理することによって
生じる塩類の溶解度が大きいことによる。In the antireflection treatment by the acid treatment method, a nitric acid solution is usually used as an acid, because the solubility of salts generated by acid treatment of glass is large.
しかしながらPbOを50％以上含有する高鉛ガラスの表
面に酸処理法によって反射防止層を形成する場合、硝酸
溶液を用いるとガラス表面に侵蝕むらが生じ、干渉色が
めだってあらわれる。また良好な全反射率を得ることが
できる最適処理条件の時間的な幅が狭いため、製造工程
における処理条件の制御が容易でなく、それゆえ歩留ま
りが悪くなるという問題が生じる。However, when an anti-reflection layer is formed on the surface of high-lead glass containing 50% or more of PbO by an acid treatment method, use of a nitric acid solution causes uneven erosion on the glass surface, and interference colors appear more noticeably. In addition, since the time width of the optimum processing conditions for obtaining a good total reflectance is narrow, it is not easy to control the processing conditions in the manufacturing process, and therefore, the yield is deteriorated.
本発明の目的は、PbOを50％以上含有し、特に大型で
厚みのある高鉛ガラスの表面に、良好な反射防止層を歩
留まりよく形成するための表面処理方法を提供すること
である。An object of the present invention is to provide a surface treatment method for forming a good antireflection layer with high yield on the surface of a large and thick high lead glass containing PbO at 50% or more.
本発明のガラス表面処理方法は、重量％でPbOを50％
以上含有する高鉛ガラスの表面を弱酸溶液で処理した
後、水洗し、加熱脱水することによって反射防止層を形
成してなることを特徴とする。The glass surface treatment method of the present invention uses 50% by weight of PbO.
The surface of the high-lead glass contained above is treated with a weak acid solution, washed with water, and heated and dehydrated to form an antireflection layer.
また本発明においては弱酸溶液が酢酸溶液であること
が好ましい。In the present invention, the weak acid solution is preferably an acetic acid solution.
本発明のガラス表面処理方法によれば、酸処理時に酢
酸溶液等の弱酸溶液を用いることにより、ガラス表面が
均一に侵蝕されるために干渉色があらわれにくい。また
良好な全反射率を得ることのできる最適処理条件の時間
点な幅が広くなり、それゆえ歩留まりが向上する。これ
らは弱酸溶液のガラス表面に対する反応が、硝酸溶液等
の強酸溶液のそれに比べて緩やかに進行することに起因
する。ところでガラスを酸処理すると、ガラス表面に近
い層中からアルカリ金属、アルカリ土類金属等が溶出
し、後にガラスより小さい屈折率を有する含水シリカ層
が残る。本発明において酸処理後のガラス表面に洗浄、
加熱脱水を行うのは前記含水シリカ層を堅牢な無水シリ
カ層とするためである。また本発明はPbOを重量％で50
％以上含有する高鉛ガラスを対象としているが、これは
以下の理由による。PbOを多量に含有するガラスは相対
的にSiO2の含有量が少ないために酸に対して弱い。しか
しながらPbOの含有量が50％より少ない場合はSiO2の含
有量が多くなり、比較的酸に対して強くなるために硝酸
溶液による処理で特に問題が生じず、あえて弱酸溶液を
使用し、長時間かけて処理する必要がない。According to the glass surface treatment method of the present invention, a weak acid solution such as an acetic acid solution is used at the time of acid treatment, so that the glass surface is uniformly eroded, so that interference colors are less likely to appear. Further, the time range of the optimum processing conditions for obtaining a good total reflectance is widened, and therefore, the yield is improved. These are due to the fact that the reaction of the weak acid solution on the glass surface progresses more slowly than that of a strong acid solution such as a nitric acid solution. By the way, when the glass is acid-treated, alkali metals, alkaline earth metals, and the like are eluted from a layer near the glass surface, and a hydrous silica layer having a refractive index smaller than that of the glass remains. In the present invention, washing the glass surface after the acid treatment,
The heat dehydration is performed to make the hydrous silica layer a robust anhydrous silica layer. Also, the present invention relates to a method in which PbO is
% Is targeted for high lead glass for the following reasons. Glass containing a large amount of PbO is weak against acids due to the relatively small content of SiO 2 . However, when the content of PbO is less than 50%, the content of SiO 2 becomes large and becomes relatively resistant to acid, so that no particular problem occurs in the treatment with a nitric acid solution. No need to process over time.
なお本発明のガラス表面処理方法においては、入手が
容易であり、かつ安価であるという点から弱酸溶液とし
ては酢酸溶液を用いるのが最も好ましいが、これ以外に
クエン酸溶液、シュウ酸溶液、硝酸アンモニウム溶液等
の弱酸溶液を使用することが可能である。In the glass surface treatment method of the present invention, it is most preferable to use an acetic acid solution as the weak acid solution because it is easily available and inexpensive, but in addition, a citric acid solution, an oxalic acid solution, and ammonium nitrate It is possible to use a weak acid solution such as a solution.
以下、本発明のガラス表面処理方法を実施例に基づい
て詳細に説明する。Hereinafter, the glass surface treatment method of the present invention will be described in detail based on examples.
まず重量％でSiO226％、B2O31％、PbO72％、K2O0.5
％、Sb2O30.5％のガラスになるように調合した原料バッ
チを石英ルツボに入れ、約1200℃で４時間溶融した後、
金型に流し込んで板状に成形した。次いで徐冷した板状
成形品を金型から取り出し、30×30×10mmの大きさに切
り出し、両面を光学研磨して試料を得た。次にこの得ら
れた試料を30℃、1/1000規定度の酢酸溶液あるいは硝酸
溶液で処理した後、水洗いし、110℃で加熱した。First, SiO 2 26%, B 2 O 3 1%, PbO 72%, K 2 O0.5
%, Sb 2 O 3 The raw material batch prepared so as to become 0.5% glass is put into a quartz crucible and melted at about 1200 ° C. for 4 hours.
It was poured into a mold and formed into a plate shape. Next, the plate-shaped molded product that was gradually cooled was taken out of the mold, cut out into a size of 30 × 30 × 10 mm, and both surfaces were optically polished to obtain a sample. Next, the obtained sample was treated with an acetic acid solution or a nitric acid solution at 30 ° C. and 1/1000 normality, washed with water, and heated at 110 ° C.
図面は、上記のようにして処理した試料一面の全反射
率と処理時間との関係を示したものである。なお処理前
の全反射率は8.3％であり、この全反射率の値が1.4％以
下になる処理時間を最適処理時間とした。The drawing shows the relationship between the total reflectance of one surface of the sample processed as described above and the processing time. The total reflectance before the processing was 8.3%, and the processing time at which the value of the total reflectance was 1.4% or less was defined as the optimum processing time.
図面から、酢酸溶液で処理した試料の最適処理時間は
約20〜25分であり、硝酸で使用した試料のそれが約２分
45秒〜３分であるのに対して時間的な幅が広いことが明
らかである。また酢酸で23分処理した試料と硝酸で２分
50秒処理した試料の表面状態を観察したところ、硝酸で
処理した試料には侵蝕むらが認められたのに対し、硝酸
で処理した試料には侵蝕むらが全く認められなかった。From the drawing, the optimal processing time of the sample treated with the acetic acid solution is about 20-25 minutes, and that of the sample used with nitric acid is about 2 minutes.
It is clear that the time range is wide compared to 45 seconds to 3 minutes. Sample treated with acetic acid for 23 minutes and nitric acid for 2 minutes
Observation of the surface condition of the sample treated for 50 seconds revealed that the sample treated with nitric acid showed uneven erosion, whereas the sample treated with nitric acid did not show any uneven erosion.
これらの事実は本発明のガラス表面処理方法がPbOを
重量％で50％以上含有する高鉛ガラスに対して、最適処
理条件の時間的な幅が広く、また全反射率が低く表面状
態のよい反射防止層を形成するのに適していることを示
している。These facts indicate that the glass surface treatment method of the present invention has a wide range of optimal treatment conditions in terms of time, high total reflectivity and good surface condition for high lead glass containing 50% by weight or more of PbO. It shows that it is suitable for forming an antireflection layer.
なお図面中の全反射率は、波長550nmにおける値を示
したものであり、150φmmの積分器をとりつけた分光光
度計を用いて、硫酸バリウムの白色拡散板を基準として
測定した。The total reflectivity in the drawings indicates a value at a wavelength of 550 nm, and was measured using a spectrophotometer equipped with an integrator of 150 mm with reference to a barium sulfate white diffusion plate.
以上のように本発明のガラス表面処理方法によるとPb
Oを重量％で50％以上含有する高鉛ガラスを酢酸溶液等
の弱酸溶液で処理することによって、良好な反射防止層
を歩留まりよく形成することが可能である。As described above, according to the glass surface treatment method of the present invention, Pb
By treating a high-lead glass containing 50% by weight or more of O with a weak acid solution such as an acetic acid solution, it is possible to form a good antireflection layer with high yield.
図面は、試料の処理時間と波長550nmにおける一面の全
反射率との関係を示したグラフであり、表中の（ａ）は
硝酸による処理、（ｂ）は酢酸による処理である。The drawing is a graph showing the relationship between the processing time of the sample and the total reflectance of one surface at a wavelength of 550 nm. In the table, (a) shows the treatment with nitric acid, and (b) shows the treatment with acetic acid.
Claims (2)
スの表面を弱酸溶液で処理した後、水洗し、加熱脱水す
ることによって反射防止層を形成してなることを特徴と
するガラス表面処理方法。1. A glass comprising a high-lead glass containing 50% by weight or more of PbO by weight, treated with a weak acid solution, washed with water, and heated and dehydrated to form an anti-reflection layer. Surface treatment method.
る特許請求の範囲第一項記載のガラス表面処理方法。2. The method according to claim 1, wherein the weak acid solution is an acetic acid solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1258224A JP2725211B2 (en) | 1989-10-02 | 1989-10-02 | Glass surface treatment method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1258224A JP2725211B2 (en) | 1989-10-02 | 1989-10-02 | Glass surface treatment method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03122030A JPH03122030A (en) | 1991-05-24 |
| JP2725211B2 true JP2725211B2 (en) | 1998-03-11 |
Family
ID=17317244
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1258224A Expired - Fee Related JP2725211B2 (en) | 1989-10-02 | 1989-10-02 | Glass surface treatment method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2725211B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811836B (en) * | 2009-02-24 | 2012-01-18 | 信义汽车玻璃(深圳)有限公司 | Method for washing and packaging of sandwich glass |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100543024B1 (en) * | 1998-01-21 | 2006-05-25 | 삼성전자주식회사 | Polarizer Removal Device of Liquid Crystal Display |
| JP3729702B2 (en) | 2000-04-13 | 2005-12-21 | 松下電器産業株式会社 | How to regenerate CRT valves |
-
1989
- 1989-10-02 JP JP1258224A patent/JP2725211B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811836B (en) * | 2009-02-24 | 2012-01-18 | 信义汽车玻璃(深圳)有限公司 | Method for washing and packaging of sandwich glass |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03122030A (en) | 1991-05-24 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |