JPH04282539A - Method for forming reflection-charge preventing film - Google Patents
Method for forming reflection-charge preventing filmInfo
- Publication number
- JPH04282539A JPH04282539A JP3044665A JP4466591A JPH04282539A JP H04282539 A JPH04282539 A JP H04282539A JP 3044665 A JP3044665 A JP 3044665A JP 4466591 A JP4466591 A JP 4466591A JP H04282539 A JPH04282539 A JP H04282539A
- Authority
- JP
- Japan
- Prior art keywords
- sio2
- film
- forming
- reflective
- glass body
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 27
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 27
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 27
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 27
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 27
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 27
- 239000011521 glass Substances 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 22
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 239000010419 fine particle Substances 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 2
- 239000011882 ultra-fine particle Substances 0.000 description 21
- 239000010410 layer Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 238000007738 vacuum evaporation Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 238000010186 staining Methods 0.000 description 2
- 241000282320 Panthera leo Species 0.000 description 1
- 230000003667 anti-reflective effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Landscapes
- Vessels, Lead-In Wires, Accessory Apparatuses For Cathode-Ray Tubes (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Formation Of Various Coating Films On Cathode Ray Tubes And Lamps (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は陰極線管、液晶表示装置
その他のディスプレイ装置のガラス表面に設ける反射・
帯電防止膜の形成に係り、特に、製造工程その他の取扱
いにおいて、汚れが付き難く、かつ、十分な実用強度を
有する反射・帯電防止膜の形成方法に関する。[Industrial Application Field] The present invention relates to a reflection device provided on the glass surface of a cathode ray tube, liquid crystal display device, or other display device.
The present invention relates to the formation of an antistatic film, and particularly to a method for forming a reflective/antistatic film that is resistant to staining during the manufacturing process and other handling processes and has sufficient strength for practical use.
【０００２】0002
【従来の技術】従来、この種の反射防止膜の形成方法と
しては真空蒸着等で多層干渉膜を積層する方法、化学エ
ッチングにより無反射膜を形成する方法などが、また、
帯電防止膜の形成方法としては真空蒸着、ＣＶＤ法など
によってＳｎＯ２、Ｉｎ２Ｏ３などからなる透明導電膜
を形成する方法などが知られているが、これらの方法を
例えば陰極線管パネル外表面の反射防止、帯電防止に適
用しようとする場合には製造コストが高くなるという問
題があった。また、完成した陰極線管にこれらの方法を
直接適用することは困難である。[Prior Art] Conventionally, methods for forming this type of antireflection film include a method of laminating a multilayer interference film by vacuum evaporation, a method of forming an antireflection film by chemical etching, etc.
As a method for forming an antistatic film, methods such as forming a transparent conductive film made of SnO2, In2O3, etc. by vacuum evaporation, CVD, etc. are known. When applied to antistatic applications, there is a problem in that the manufacturing cost becomes high. Furthermore, it is difficult to directly apply these methods to completed cathode ray tubes.
【０００３】これらの問題点に対して、本発明者等は、
先に、ＳｉＯ２の超微粒子を添加したＳｉ（ＯＲ）４（
Ｒはアルキル基）のアルコール溶液をガラス体表面に塗
布、焼成して、該ガラス体の表面上にＳｉＯ２超微粒子
とこれを接着するＳｉＯ２バインダとからなる反射防止
膜を形成する方法を提案した（特開昭６３‐１９３１０
１号）。また、上記組成の塗布液にそれ自体が導電性を
有するＳｎＯ２、Ｉｎ２Ｏ３の超微粒子を含有させるこ
とによって、帯電防止効果を付与した反射防止膜につい
ても提案した（特開平０１‐１５４４４４号）。[0003] In response to these problems, the present inventors have
First, Si(OR)4(
We proposed a method of coating an alcoholic solution of R (alkyl group) on the surface of a glass body and firing it to form an antireflection film on the surface of the glass body, which consists of ultrafine SiO2 particles and a SiO2 binder that adheres them. Japanese Patent Publication No. 63-19310
No. 1). They also proposed an antireflection film that imparts an antistatic effect by incorporating ultrafine particles of SnO2 and In2O3, which themselves have conductivity, into a coating solution having the above composition (Japanese Patent Laid-Open No. 154444/1999).
【０００４】0004
【発明が解決しようとする課題】上記本発明者等提案の
方法は、ガラス体表面の他に、従来技術では困難であっ
た陰極線管パネルの外表面に反射・帯電防止膜を直接形
成できるという優れた効果を有する方法であるが、該反
射・帯電防止膜の表面を手で触れたりすると指紋などの
汚れが付きやすく、また、この汚れが容易に除去できる
ものではないために、反射防止特性を損なうことがあっ
た。また、ここで得られる反射・帯電防止膜の構成粒子
同士の接着強度および該膜とガラス体表面との間の接着
強度が小さいために、硬いもので摩擦するようなことが
起った場合に、構成粒子の一部が削り取られたりあるい
はガラス体表面から一部剥離してしまうことがあった。
例えば、消しゴム（ライオン事務器製、タイプ５０‐５
０）で擦った場合にもこのような現象が発生していた。[Problems to be Solved by the Invention] The method proposed by the present inventors can directly form a reflective and antistatic film on the outer surface of the cathode ray tube panel, which was difficult to do with conventional techniques, in addition to the surface of the glass body. Although this method has excellent effects, when the surface of the reflective/antistatic coating is touched with hands, fingerprints and other stains are likely to adhere, and since this stain cannot be easily removed, the antireflective properties may be damaged. In addition, since the adhesive strength between the constituent particles of the reflective/antistatic film obtained here and the adhesive strength between the film and the surface of the glass body are low, when friction occurs with a hard object, In some cases, some of the constituent particles were scraped off or partially peeled off from the surface of the glass body. For example, eraser (manufactured by Lion Office Equipment, type 50-5)
0), such a phenomenon also occurred.
【０００５】本発明の目的は、上記従来技術の有してい
た課題を解決して、製造工程その他の取扱いにおいて、
汚れが付き難く、かつ、十分な実用強度を有する反射・
帯電防止膜の形成方法を提供することにある。An object of the present invention is to solve the problems of the above-mentioned prior art, and to improve the manufacturing process and other handling.
Reflective material that is hard to get dirty and has sufficient strength for practical use.
An object of the present invention is to provide a method for forming an antistatic film.
【０００６】[0006]
【発明を解決するための手段】上記目的は、ＳｉＯ２超
微粒子とＳｎＯ２超微粒子とを添加したＳｉ（ＯＲ）４
のアルコール溶液をディップ法あるいはスピン法により
ガラス体表面上に塗布して反射・帯電防止膜を形成した
後、該膜上にさらにＳｉ（ＯＲ）４のアルコール溶液を
ディップ法により塗布、焼成してＳｉＯ２膜層を形成す
ることによって達成することができる。Means for Solving the Invention The above object is to provide Si(OR)4 to which SiO2 ultrafine particles and SnO2 ultrafine particles are added.
An alcohol solution of Si(OR)4 is applied onto the surface of the glass body by a dip method or a spin method to form a reflective/antistatic film, and then an alcohol solution of Si(OR)4 is further applied onto the film by a dip method and baked. This can be achieved by forming a SiO2 film layer.
【０００７】[0007]
【作用】上記したようにガラス体表面上に形成した、Ｓ
ｉＯ２超微粒子とＳｎＯ２超微粒子およびこれらを接着
固定するためのＳｉＯ２バインダからなる反射・帯電防
止膜上にさらにＳｉＯ２層を形成すると、後者のＳｉＯ
２層が前者の反射・帯電防止膜の保護層の役目を果し、
これによって、反射・帯電防止膜の耐汚染性、耐摩耗性
に関する実用強度を確保することができる。[Operation] S formed on the surface of the glass body as described above.
When an SiO2 layer is further formed on the reflection/antistatic film made of iO2 ultrafine particles, SnO2 ultrafine particles, and a SiO2 binder for adhering and fixing them, the latter SiO
The two layers serve as a protective layer for the former reflective/antistatic film,
This makes it possible to ensure practical strength in terms of stain resistance and abrasion resistance of the reflective/antistatic film.
【０００８】上記本発明の方法によって形成した反射・
帯電防止膜と従来技術の方法による反射・帯電防止膜と
の比較について、図によってさらに詳細に説明すれば次
の通りである。Reflections formed by the method of the present invention described above
A comparison between the antistatic film and the reflective/antistatic film formed by the prior art method will be explained in more detail with reference to the drawings as follows.
【０００９】まず、図２は従来技術の方法によって形成
した反射・帯電防止膜４の構成状態を示す断面図で、こ
の場合、ＳｉＯ２超微粒子１は反射防止効果を、ＳｎＯ
２超微粒子２は導電性を、また、ＳｉＯ２バインダ３は
ＳｉＯ２超微粒子１とＳｎＯ２超微粒子２およびガラス
体表面５との接着固定の役割を果す。ここで、ＳｉＯ２
超微粒子１として平均粒径１２０ｎｍの粒子を用いた場
合、凹凸の深さは約６０〜１２０ｎｍで、極めて微細な
凹凸となる。また、このような場合、ＳｉＯ２超微粒子
１とＳｎＯ２超微粒子２とガラス体表面５とは殆ど点で
接着している。このような状態の表面を手で触れたり、
消しゴム等の硬い物で擦ったりすると、汚れが付いたり
、消しゴムかすが凹凸の間に埋まったりするため汚れが
取れ難くなったり、ＳｉＯ２、ＳｎＯ２超微粒子がガラ
ス体表面５から剥離したり、または、ＳｉＯ２超微粒子
が摩耗したりするために、反射防止効果が損なわれるこ
とがある。First, FIG. 2 is a cross-sectional view showing the configuration of a reflection/antistatic coating 4 formed by a conventional method.
2 The ultrafine particles 2 have conductivity, and the SiO2 binder 3 serves to bond and fix the SiO2 ultrafine particles 1, the SnO2 ultrafine particles 2, and the glass body surface 5. Here, SiO2
When particles with an average particle diameter of 120 nm are used as the ultrafine particles 1, the depth of the unevenness is approximately 60 to 120 nm, resulting in extremely fine unevenness. Further, in such a case, the SiO2 ultrafine particles 1, the SnO2 ultrafine particles 2, and the glass body surface 5 are adhered at almost all points. Do not touch the surface in this condition with your hands,
If you rub it with a hard object such as an eraser, it will get dirty, or the eraser scum will get buried between the unevenness, making it difficult to remove the dirt, or the ultrafine particles of SiO2 and SnO2 will peel off from the surface of the glass body 5, or the SiO2 The antireflection effect may be impaired due to wear of the ultrafine particles.
【００１０】これに対して、図１は本発明の方法により
形成した反射・帯電防止膜の概略構成を示した図で、こ
の場合には、従来技術の場合と同様構成の反射・帯電防
止膜の上にさらにＳｉＯ２層６（厚さ約５〜２０ｎｍ）
が反射防止特性を劣化させることなく設けられているた
めに、ＳｉＯ２超微粒子、ＳｎＯ２超微粒子同士および
ガラス体表面とが十分に接着固定することができるため
、耐汚染性、耐摩耗性に関して十分な実用強度を確保す
ることができる。On the other hand, FIG. 1 is a diagram showing a schematic structure of a reflective/antistatic film formed by the method of the present invention. Further SiO2 layer 6 (thickness approximately 5-20 nm)
is provided without deteriorating the antireflection properties, and the SiO2 ultrafine particles and SnO2 ultrafine particles can be sufficiently adhesively fixed to each other and to the glass body surface, resulting in sufficient stain resistance and abrasion resistance. Practical strength can be ensured.
【００１１】ＳｉＯ２層の形成はスピン塗布法あるいは
スプレー塗布法によって行うこともできるが、反射防止
特性を損なうことがあるため不適である。また、真空蒸
着法で形成することも可能であるが、完成した陰極線管
などの大きなものに適用するためには大がかりな設備を
必要とするため、製造コストの点から方法としては不適
である。これらのことから、ＳｉＯ２層６の形成にはデ
ィップ法が最適である。[0011] The SiO2 layer can be formed by spin coating or spray coating, but this is not suitable because it may impair the antireflection properties. It is also possible to form the film by vacuum evaporation, but it requires large-scale equipment to be applied to large objects such as completed cathode ray tubes, making it unsuitable as a method in terms of manufacturing costs. For these reasons, the dipping method is most suitable for forming the SiO2 layer 6.
【００１２】なお、ガラス体の表面にＳｉＯ２超微粒子
膜を形成することによって反射防止効果が得られるのは
、空気の屈折率を１．０、ＳｉＯ２超微粒子の屈折率を
１．４８としたとき、ＳｉＯ２超微粒子の凹凸形状部分
において屈折率がＳｉＯ２の体積分律に従って連続的に
変化することによる反射低減効果によるものである。ま
た、導電性はＳｎＯ２超微粒子自体の電子伝導性による
ものである。[0012] The antireflection effect can be obtained by forming a SiO2 ultrafine particle film on the surface of a glass body when the refractive index of air is 1.0 and the refractive index of SiO2 ultrafine particles is 1.48. This is due to the reflection reduction effect caused by the refractive index continuously changing in the uneven portion of the SiO2 ultrafine particles according to the volumetric law of SiO2. Further, the conductivity is due to the electronic conductivity of the SnO2 ultrafine particles themselves.
【００１３】[0013]
【実施例】以下、本発明方法の内容について比較例との
比較によって具体的に説明する。EXAMPLES The content of the method of the present invention will be specifically explained below by comparison with comparative examples.
【００１４】まず反射・帯電防止膜を形成すべきガラス
体の表面を研摩材及びアルカリ洗浄剤等を用いて清浄化
した後、表１に示した反射・帯電防止膜塗布液およびＳ
ｉＯ２層形成塗布液を該ガラス体表面上に塗布し、１５
０℃３０分間の焼成を行った。すなわち、実施例１、２
及び比較例１、２においては、反射・帯電防止膜塗布液
をガラス体引上げ速度０．５ｍｍ／秒でディップ塗布、
実施例３においては回転数２００ｒｐｍでスピン塗布を
行った。続いて、実施例１、３についてはＳｉＯ２層形
成塗布液をガラス体引上げ速度０．５ｍｍ／秒で、実施
例２についてはガラス体引上げ速度０．８ｍｍ／秒でデ
ィップ塗布、比較例１については回転数２００ｒｐｍで
スピン塗布を行った。最後に上記各試料を１５０℃３０
分間焼成した物を試料として、反射特性、耐摩耗性及び
汚染除去性を調べた。結果を表１膜特性の欄に示した。First, the surface of the glass body on which the reflective/antistatic film is to be formed is cleaned using an abrasive and an alkaline cleaning agent, and then the reflective/antistatic film coating solution and S shown in Table 1 are applied.
Applying an iO2 layer forming coating liquid onto the surface of the glass body,
Firing was performed at 0°C for 30 minutes. That is, Examples 1 and 2
In Comparative Examples 1 and 2, the reflective/antistatic film coating solution was dip coated at a glass body pulling speed of 0.5 mm/sec.
In Example 3, spin coating was performed at a rotation speed of 200 rpm. Subsequently, for Examples 1 and 3, the SiO2 layer forming coating solution was applied by dip coating at a glass body pulling rate of 0.5 mm/sec, for Example 2, a glass body pulling rate of 0.8 mm/sec, and for Comparative Example 1, Spin coating was performed at a rotation speed of 200 rpm. Finally, each sample was heated to 30°C at 30°C.
Reflection properties, abrasion resistance, and stain removability were investigated using samples baked for minutes. The results are shown in the membrane properties column of Table 1.
【００１５】表１の結果から、比較例１の試料は初期の
反射特性が悪く、比較例２の試料は耐摩耗性が小さくま
た汚れ除去性も悪いのに対して、本発明実施例１、２、
３の試料は何れも初期の反射特性が良く、耐摩耗強度も
強く、汚れ除去性も極めて容易であることが判る。なお
、上記汚れ除去性の検査は、反射・帯電防止膜を指で触
って指紋を付けた後メタノールで拭きとり、そのときの
指紋の除去し易さの比較によって行った。また、本発明
実施例試料の反射・帯電防止膜の表面抵抗の初期値は何
れも１×１０９Ω／□であり、十分高い導電性を示すも
のであった。From the results in Table 1, it can be seen that the sample of Comparative Example 1 had poor initial reflection characteristics, and the sample of Comparative Example 2 had low abrasion resistance and poor dirt removal properties, whereas the sample of Example 1 of the present invention, 2,
It can be seen that all samples No. 3 have good initial reflection characteristics, strong abrasion resistance, and are extremely easy to remove dirt. The stain removability was tested by touching the reflective/antistatic film with a finger to leave a fingerprint on it, then wiping it off with methanol, and comparing the ease with which the fingerprint was removed. Further, the initial values of the surface resistance of the reflective/antistatic coatings of the samples of the examples of the present invention were all 1×10 9 Ω/□, indicating sufficiently high conductivity.
【００１６】[0016]
【表１】[Table 1]
【００１７】[0017]
【発明の効果】以上述べてきたように、反射・帯電防止
膜の形成方法を本発明の形成方法とすることによって、
従来技術の有していた課題を解決して、製造工程その他
の取扱いにおいて汚れが付き難く、かつ、十分な実用強
度を有する反射・帯電防止膜の形成方法を提供すること
ができた。この方法によって、上記の優れた特性を有す
る反射・帯電防止膜を簡単な工程で、低コストで得るこ
とができる。[Effects of the Invention] As described above, by using the method of forming a reflective/antistatic film according to the present invention,
By solving the problems of the prior art, it has been possible to provide a method for forming a reflective/antistatic film that is resistant to staining during the manufacturing process and other handling processes and has sufficient strength for practical use. By this method, a reflective/antistatic film having the above-mentioned excellent properties can be obtained through simple steps and at low cost.
【図１】図１は本発明の方法で形成した反射・帯電防止
膜の断面構造を示す模式図。FIG. 1 is a schematic diagram showing the cross-sectional structure of a reflective/antistatic film formed by the method of the present invention.
【図２】図２は従来技術の方法で形成した反射・帯電防
止膜の断面構造を示す模式図。FIG. 2 is a schematic diagram showing the cross-sectional structure of a reflective/antistatic film formed by a conventional method.
１…ＳｉＯ２超微粒子、２…ＳｎＯ２超微粒子、３…Ｓ
ｉＯ２バインダ、４…反射・帯電防止膜、５…ガラス体
、６…ＳｉＯ２層。1...SiO2 ultrafine particles, 2...SnO2 ultrafine particles, 3...S
iO2 binder, 4... reflective/antistatic film, 5... glass body, 6... SiO2 layer.
Claims (1)
したＳｉ（ＯＲ）４（Ｒはアルキル基）のアルコール溶
液をディップ法あるいはスピン法によりガラス体表面上
に塗布して反射・帯電防止膜を形成した後、該膜上にさ
らにＳｉ（ＯＲ）４のアルコール溶液をディップ法によ
り塗布、焼成してＳｉＯ２膜層を形成したことを特徴と
する反射・帯電防止膜の形成方法。Claim 1: A reflective/antistatic film is formed by applying an alcoholic solution of Si(OR)4 (R is an alkyl group) to which SiO2 fine particles and SnO2 fine particles are added onto the surface of a glass body using a dipping method or a spin method. After that, an alcohol solution of Si(OR)4 is further coated on the film by a dip method and baked to form a SiO2 film layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3044665A JPH04282539A (en) | 1991-03-11 | 1991-03-11 | Method for forming reflection-charge preventing film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3044665A JPH04282539A (en) | 1991-03-11 | 1991-03-11 | Method for forming reflection-charge preventing film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04282539A true JPH04282539A (en) | 1992-10-07 |
Family
ID=12697746
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3044665A Pending JPH04282539A (en) | 1991-03-11 | 1991-03-11 | Method for forming reflection-charge preventing film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04282539A (en) |
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- 1991-03-11 JP JP3044665A patent/JPH04282539A/en active Pending
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