JPH0692623A - Heat-resistant transparent yellow film and composition for forming the same film - Google Patents
Heat-resistant transparent yellow film and composition for forming the same filmInfo
- Publication number
- JPH0692623A JPH0692623A JP33291291A JP33291291A JPH0692623A JP H0692623 A JPH0692623 A JP H0692623A JP 33291291 A JP33291291 A JP 33291291A JP 33291291 A JP33291291 A JP 33291291A JP H0692623 A JPH0692623 A JP H0692623A
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- Prior art keywords
- film
- vanadium pentoxide
- heat
- weight ratio
- composition
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- Surface Treatment Of Glass (AREA)
- Glass Compositions (AREA)
- Silicon Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、紫外線による劣化を防
ぐためのコーティングや、車輛、船舶等の照明用ハロゲ
ンランプあるいは警報ランプ等の透明着色膜としてこれ
らの透明ガラス器材の表面に形成される高耐熱性透明黄
色膜に関し、さらに該被膜を形成するための組成物に関
する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is formed on the surface of transparent glass equipment as a coating for preventing deterioration due to ultraviolet rays, or as a transparent colored film for halogen lamps for lighting vehicles, ships, etc. or alarm lamps. It relates to a highly heat-resistant transparent yellow film, and further to a composition for forming the film.
【０００２】[0002]
【従来技術とその課題】着色被膜の形成法としては、従
来から、静電塗装法、スパッタリング法、ＣＶＤ法、被
膜液の塗布法等が知られているが、耐熱性黄色透明体を
得るためにはそれぞれ問題がある。静電塗装法は塗布材
の粒径を最適にする制御が困難で、しかも粒子が凝集し
やすく、そのため光の散乱が起りやすく透明性が劣る。
またスパッタリング法やＣＶＤ法は高価な装置が必要な
うえに生産性が良くない。一方、塗布法は生産性が良
く、均質な被膜を容易に形成でき、組成の制御も容易で
あるが、従来知られている黄色系塗膜形成用組成物は耐
熱性に劣る問題がある。例えば、従来、セリウム含有酸
化チタン(特開昭61-34185号、同63-103083号)、鉄酸化
物とチタン酸化物との系にコバルト、クロム、ジルコニ
ウム、スズ等を必要に応じて含有させたもの(特開昭54-
101821号)、0.1μm以下の酸化亜鉛等を溶剤もしくは結
合剤中に分散したもの等(特開平2-169673号、同2-26597
6号)が知られているが、これらの膜は約500℃前後の高
温下では耐熱性に乏しい。本発明者は、高温環境下で使
われる耐熱ガラスを、紫外線の遮断あるいは着色を目的
として表面コーティングするために各種材料たとえば、
Pb-Zr-Cr-O、 Zr-Si-Pr-O、Ti-Sb-Ni-Nb-O、Ti-Fe-Zn-O
等について検討した。しかしいずれも吸光係数が小さ
く、着色薄膜としては有効でなかったり、あるいは高温
環境下ではすぐに劣化する欠点があり、耐熱性着色被膜
として不十分であった。2. Description of the Related Art Electrostatic coating method, sputtering method, CVD method, coating method of coating liquid, etc. have been known as a method for forming a colored coating film. There are problems with each. In the electrostatic coating method, it is difficult to control the particle size of the coating material to be optimum, and moreover, the particles are likely to agglomerate, so that light scattering is likely to occur and the transparency is poor.
Further, the sputtering method and the CVD method require expensive equipment and are not good in productivity. On the other hand, the coating method has high productivity, can easily form a uniform coating film, and can easily control the composition, but the conventionally known yellow coating film forming composition has a problem of poor heat resistance. For example, conventionally, cerium-containing titanium oxide (JP-A-61-34185, JP-A-63-103083), cobalt, chromium, zirconium, tin and the like as needed to the system of iron oxide and titanium oxide. Tamono (Japanese Patent Laid-Open No. 54-
101821), 0.1 μm or less zinc oxide or the like dispersed in a solvent or a binder, etc. (JP-A-2-169673, 2-26597)
No. 6) is known, but these films have poor heat resistance at high temperatures around 500 ° C. The present inventor has made various materials such as heat-resistant glass used under a high temperature environment for surface coating for the purpose of blocking or coloring ultraviolet rays, for example,
Pb-Zr-Cr-O, Zr-Si-Pr-O, Ti-Sb-Ni-Nb-O, Ti-Fe-Zn-O
Etc. were examined. However, each of them has a small extinction coefficient, is not effective as a colored thin film, or has a defect that it is easily deteriorated in a high temperature environment, and is insufficient as a heat resistant colored coating.
【０００３】[0003]
【発明の解決課題】本発明は、従来の上記課題を解決し
た高耐熱性の透明黄色膜と該被膜形成用組成物を提供す
ることを目的とする。本発明者は、高耐熱性の黄色透明
膜と該被膜形成用組成物について検討を続けた結果、シ
リコン−バナジウム系酸化物が、従来の被膜より耐熱性
の一段と優れた黄色系透明被膜を形成することを見い出
した。SUMMARY OF THE INVENTION It is an object of the present invention to provide a highly heat-resistant transparent yellow film and a composition for forming the film, which solves the above-mentioned conventional problems. The present inventor, as a result of continuing studies on a high heat-resistant yellow transparent film and the composition for forming a film, a silicon-vanadium oxide forms a yellow-based transparent film which is more excellent in heat resistance than a conventional film. I found out what to do.
【０００４】[0004]
【課題の解決手段：発明の構成】本発明によれば、シリ
カ中に、微細な五酸化バナジウムがＳｉＯ2／Ｖ2Ｏ5重
量比で1.5〜3.5の範囲に均一に分散した耐熱性黄色透明
膜が提供される。さらに本発明によれば、アルキルシリ
ケートまたはシリカゾルの溶液中に粒径0.2μm以下の五
酸化バナジウム粉末が均一に分散された黄色膜形成用組
成物であって、五酸化バナジウム粉末の含有量が、形成
された膜中のＳｉＯ2／Ｖ2Ｏ5 重量比で1.5〜3.5となる
範囲であることを特徴とする耐熱性透明黄色膜形成用組
成物が提供される。According to the present invention, according to the present invention, fine vanadium pentoxide is uniformly dispersed in a range of 1.5 to 3.5 in terms of SiO 2 / V 2 O 5 weight ratio in heat-resistant yellow transparent. A membrane is provided. Furthermore, according to the present invention, a yellow film-forming composition in which vanadium pentoxide powder having a particle size of 0.2 μm or less is uniformly dispersed in a solution of alkyl silicate or silica sol, wherein the content of vanadium pentoxide powder is There is provided a heat-resistant transparent yellow film-forming composition, wherein the SiO 2 / V 2 O 5 weight ratio in the formed film is in the range of 1.5 to 3.5.
【０００５】本発明の被膜は、ガラス状のＳｉＯ2中
に、微細な五酸化バナジウムがＳｉＯ2／Ｖ2Ｏ5重量比
で1.5〜3.5となる範囲に均一に分散した耐熱性の透明黄
色膜である。ここでＳｉＯ2／Ｖ2Ｏ5の重量比が1.5未満
であると、高温環境下では五酸化バナジウムの粒成長が
起り透明性が失われる。また耐熱性が得られない。一
方、ＳｉＯ2／Ｖ2Ｏ5の重量比が3.5を越えると、五酸化
バナジウムの量が相対的に少なく、着色力が弱くなるた
め好ましくない。五酸化バナジウムは、粒径0.2μm以下
の微粒子であることが好ましい。0.2μmより粒径が大き
いと被膜の透明性が低下する。一方五酸化バナジウムの
粒径が0.2μm以下であるとき、約500nm以下の波長を効
率よく吸収し、かつそれ以上の波長では透明性の非常に
良い被膜を得ることができる。[0005] Coatings of the present invention, in the glass-like SiO 2, fine vanadium pentoxide is homogeneously dispersed in the range of a 1.5 to 3.5 at a SiO 2 / V 2 O 5 weight ratio heat resistance of the transparent yellow film Is. If the weight ratio of SiO 2 / V 2 O 5 is less than 1.5, vanadium pentoxide grain growth occurs in a high temperature environment and the transparency is lost. In addition, heat resistance cannot be obtained. On the other hand, if the weight ratio of SiO 2 / V 2 O 5 exceeds 3.5, the amount of vanadium pentoxide is relatively small and the coloring power becomes weak, which is not preferable. Vanadium pentoxide is preferably fine particles having a particle size of 0.2 μm or less. If the particle size is larger than 0.2 μm, the transparency of the coating film will decrease. On the other hand, when the particle size of vanadium pentoxide is 0.2 μm or less, it is possible to efficiently absorb a wavelength of about 500 nm or less, and to obtain a highly transparent coating film at a wavelength of more than that.
【０００６】本発明の被膜は、溶液法(ゾルゲル法)、CV
D法、スパッタリング法など通常の方法によって形成す
ることができる。CVD法の一例としては、耐熱性透明基
体を装入した密閉容器内にテトラエトキシオルソシラン
(TEOS)とトリエトキシバナジルの原料ガスを供給し、Ｓ
ｉＯ2／Ｖ2Ｏ5重量比1.5〜3.5の範囲に調製して透明基
体表面に上記被膜を気相成長させる。またスパッタリン
グ法による場合には、予めＳｉＯ2／Ｖ2Ｏ5重量比1.5〜
3.5のスパッタ用ターゲットを作成し、これを用いて耐
熱性透明基体表面に上記被膜を形成することができる。
溶液法に用いる組成物としては、アルキルシリケート又
はシリカゾルの溶液中に粒径0.2μm以下の五酸化バナジ
ウム粉末が均一に分散された組成物であって、五酸化バ
ナジウム粉末の含有量が、形成された膜中のＳｉＯ2／
Ｖ2Ｏ5 重量比で1.5〜3.5となる範囲であることを特徴
とする耐熱性透明黄色膜形成用組成物が好適に用いられ
る。The coating film of the present invention is a solution method (sol-gel method), CV
It can be formed by an ordinary method such as D method or sputtering method. As an example of the CVD method, tetraethoxy orthosilane is placed in a closed container containing a heat-resistant transparent substrate.
(TEOS) and triethoxyvanadyl source gas are supplied, and S
The iO 2 / V 2 O 5 weight ratio is adjusted to a range of 1.5 to 3.5 to vapor-deposit the above coating on the surface of the transparent substrate. When the sputtering method is used, the SiO 2 / V 2 O 5 weight ratio is 1.5 to
It is possible to form a sputtering target of 3.5 and use it to form the above coating on the surface of the heat-resistant transparent substrate.
The composition used in the solution method is a composition in which vanadium pentoxide powder having a particle size of 0.2 μm or less is uniformly dispersed in a solution of alkyl silicate or silica sol, and the content of vanadium pentoxide powder is formed. SiO 2 in the film
A heat-resistant transparent yellow film-forming composition having a V 2 O 5 weight ratio of 1.5 to 3.5 is preferably used.
【０００７】溶液法に用いる上記組成物溶液の二酸化ケ
イ素源は、高温環境下での使用を目的として、アルキル
シリケートあるいはシリカゾルが使用される。アルキル
シリケートは任意に選択することがでる。具体的には、
例えば、テトラエトキシオルソシラン(TEOS)、テトラメ
チルオルソシラン(TMOS)、テトラプロピルオルソシラン
(TPOS)、テトラブチルオルソシラン(TBOS)、メチルエト
キシシラン(MTES)、ジメチルジエトキシシランなどの単
体またはこれらの混合物が用いられる。アルキルシリケ
ートを用いる場合には、例えばアルキルシリケートをア
ルコール等の溶剤に溶解した後に稀塩酸を加えて部分加
水分解し、生成する固形物(SiO2)が適当な濃度となるよ
うにアルコール等により濃度を調整して用いるのが好ま
しい。As the silicon dioxide source of the above composition solution used in the solution method, an alkyl silicate or silica sol is used for the purpose of use in a high temperature environment. The alkyl silicate can be arbitrarily selected. In particular,
For example, tetraethoxy orthosilane (TEOS), tetramethyl orthosilane (TMOS), tetrapropyl orthosilane
(TPOS), tetrabutylorthosilane (TBOS), methylethoxysilane (MTES), dimethyldiethoxysilane, etc., or a mixture thereof is used. In the case of using an alkyl silicate, for example, the alkyl silicate is dissolved in a solvent such as alcohol and then diluted with dilute hydrochloric acid to partially hydrolyze the solution, and the resulting solid matter (SiO 2 ) is concentrated with alcohol or the like so as to have an appropriate concentration. Is preferably adjusted before use.
【０００８】上記組成物溶液に混合する五酸化バナジウ
ム微粉末の量は、形成された膜中のＳｉＯ2／Ｖ2Ｏ5重
量比が1.5〜3.5となる範囲である。組成物溶液中に五酸
化バナジウム微粉末を均一に分散させる方法は制限され
ない。例えばボールミル等通常の混合装置が使用でき
る。なお混合する場合には十分に時間をかけて五酸化バ
ナジウム粉末を組成物溶液中に均一に分散させることが
好ましい。分散が不十分であると、500℃以上の高温環
境下で五酸化バナジウムの粒成長が容易に起り短時間で
膜の白濁、失透を生じ耐熱効果が得られない。本発明の
上記組成物溶液を耐熱ガラスなどの透明基体の片面また
は両面に塗布して加熱し、加熱分解することにより高耐
熱性黄色透明体が得られる。塗膜の厚さ、塗布方法およ
び加熱方法は常法に準じて行えばよい。形成された被膜
は黄色系の色調を有する透明被膜であり、500℃以上の
高温環境下でも色調および透明度が変化しない。The amount of the vanadium pentoxide fine powder to be mixed with the above composition solution is in a range such that the SiO 2 / V 2 O 5 weight ratio in the formed film is 1.5 to 3.5. The method of uniformly dispersing vanadium pentoxide fine powder in the composition solution is not limited. For example, a usual mixing device such as a ball mill can be used. In the case of mixing, it is preferable that the vanadium pentoxide powder is uniformly dispersed in the composition solution for a sufficient time. If the dispersion is insufficient, the grain growth of vanadium pentoxide easily occurs in a high temperature environment of 500 ° C. or higher, causing clouding and devitrification of the film in a short time, and the heat resistance effect cannot be obtained. A highly heat-resistant yellow transparent body is obtained by applying the composition solution of the present invention to one or both sides of a transparent substrate such as heat-resistant glass, heating, and thermally decomposing it. The thickness of the coating film, the coating method and the heating method may be carried out according to the usual methods. The formed film is a transparent film having a yellowish color tone, and the color tone and transparency do not change even in a high temperature environment of 500 ° C or higher.
【０００９】[0009]
【発明の効果】本発明のＳｉＯ2／Ｖ2Ｏ5系被膜は、高
耐熱性および透明性に優れた黄色膜であり、この被膜を
有する耐熱ガラス製の照明用ハロゲンランプや警報ラン
プ等は高耐熱性を有し、高温下での使用に適する。また
上記被膜形成用組成物は照明用ハロゲンランプや警報ラ
ンプ等の透明基材に塗布して加熱するだけで容易に高耐
熱性の透明黄色膜を形成できる。The SiO 2 / V 2 O 5 type coating film of the present invention is a yellow film excellent in high heat resistance and transparency, and a halogen lamp for lighting or an alarm lamp made of heat resistant glass having this coating film It has high heat resistance and is suitable for use at high temperatures. Further, a highly heat-resistant transparent yellow film can be easily formed simply by applying the coating composition to a transparent substrate such as a halogen lamp for illumination or an alarm lamp and heating it.
【０００１０】実施例１ テトラエトキシオルソシラン(TEOS)5.00gをイソプロパ
ノールに溶かし、稀塩酸を加え部分加水分解をした後、
固形物(SiO2)重量が10％濃度となるようにイソプロパノ
ールで濃度調整を行い結合剤溶液とした。この溶液10g
中に粒径0.05μm以下の五酸化バナジウム微粉末0.4gを
加えて良く混合し、ボールミルで100時間攪拌して五酸
化バナジウム微粉末を均一分散させ膜形成用組成物を得
た。この組成物をディッピング法でバイコールガラスに
塗布し、加熱乾燥してＸＹＺ表色系の色度(ｘ，ｙ)＝
(0.498,0.448)、Ｙ＝85.1の黄色着色透明体を得た。こ
の着色体を700℃の高温で保特した際のＹ値は図１に示
すように殆ど変化せず、膜の白濁、失透もない高温耐熱
性に優れたものであった。Example 1 Tetraethoxy orthosilane (TEOS) (5.00 g) was dissolved in isopropanol, diluted hydrochloric acid was added for partial hydrolysis, and
The concentration was adjusted with isopropanol so that the weight of the solid matter (SiO 2 ) was 10% to obtain a binder solution. 10 g of this solution
0.4 g of vanadium pentoxide fine powder having a particle size of 0.05 μm or less was added and well mixed, and the mixture was stirred for 100 hours with a ball mill to uniformly disperse the vanadium pentoxide fine powder to obtain a film-forming composition. This composition was applied to Vycor glass by a dipping method and dried by heating to obtain the chromaticity (x, y) of XYZ color system =
(0.498, 0.448), Y = 85.1, a yellow colored transparent body was obtained. When this colored body was maintained at a high temperature of 700 ° C., the Y value hardly changed as shown in FIG. 1, and the film was excellent in high temperature heat resistance without clouding or devitrification.
【００１１】実施例２ テトラエトキシオルソシラン(TEOS)5.00gをイソプロパ
ノールに溶かし、稀塩酸を加え部分加水分解をした後、
固形物(SiO2)重量が10％濃度となるようにイソプロパノ
ールで濃度調整を行い組成物溶液とした。この溶液10g
中に粒径0.05μm以下の五酸化バナジウム微粉末0.5gを
加えて良く混合し、ボールミルで100時間攪拌して五酸
化バナジウム微粉末を均一分散させ膜形成用組成物を得
た。この組成物をディッピング法でバイコールガラスに
塗布し、加熱乾燥してＸＹＺ表色系の色度(ｘ，ｙ)＝
(0.504,0.449)、Ｙ＝84.8の黄色着色透明体を得た。こ
の着色体を700℃の高温で保持した際の耐熱性は実施例
１と同様であった。Example 2 Tetraethoxy orthosilane (TEOS) (5.00 g) was dissolved in isopropanol, diluted hydrochloric acid was added to the mixture for partial hydrolysis, and
The concentration was adjusted with isopropanol so that the weight of the solid matter (SiO 2 ) would be 10% to obtain a composition solution. 10 g of this solution
0.5 g of vanadium pentoxide fine powder having a particle size of 0.05 μm or less was added and well mixed, and the mixture was stirred for 100 hours in a ball mill to uniformly disperse the vanadium pentoxide fine powder to obtain a film-forming composition. This composition was applied to Vycor glass by a dipping method and dried by heating to obtain the chromaticity (x, y) of XYZ color system =
(0.504, 0.449), Y = 84.8, a yellow colored transparent body was obtained. The heat resistance of this colored body when held at a high temperature of 700 ° C. was similar to that of Example 1.
【００１２】比較例１ 実施例１と同様にして膜形成用組成物を作製した。但
し、ボールミルによる均一分散時間は10分しか行わなか
った。この組成物を実施例１と同様にしてバイコールガ
ラスに塗布し、ＸＹＺ表色系の色度(ｘ，ｙ)＝(0.496,
0.4538)、Ｙ＝79.4の黄色着色透明体を得た。この着色
体を700℃の高温で保持した際のＹ値変化を図２に示
す。図示するように本例の着色体は短時間で膜の白濁、
失透が起こり耐熱性が劣るものであった。これは実施例
１と比較して五酸化バナジウムの分散性が悪く、容易に
粒成長を起こすためであると考えられる。Comparative Example 1 A film forming composition was prepared in the same manner as in Example 1. However, the uniform dispersion time by the ball mill was only 10 minutes. This composition was applied to Vycor glass in the same manner as in Example 1, and the chromaticity (x, y) of the XYZ color system = (0.496,
0.4538), Y = 79.4 to obtain a yellow colored transparent body. FIG. 2 shows the change in Y value when the colored body was held at a high temperature of 700 ° C. As shown in the figure, the colored body of this example shows a cloudiness of the film in a short time,
Devitrification occurred and heat resistance was poor. It is considered that this is because the dispersibility of vanadium pentoxide was poor as compared with Example 1 and grain growth was easily caused.
【図１】 実施例１で得た本発明の着色体を700℃に保
持した際のＹ値の経時変化を示す図。FIG. 1 is a diagram showing a change with time of a Y value when the colored body of the present invention obtained in Example 1 is held at 700 ° C.
【図２】 比較例１で得た着色体を700℃に保持した際
のＹ値の経時変化を示す図。FIG. 2 is a view showing a change with time of a Y value when the colored body obtained in Comparative Example 1 is kept at 700 ° C.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 佐藤 勇 東京都目黒区中目黒２丁目９番13号 スタ ンレー電気株式会社内 ─────────────────────────────────────────────────── ─── Continued Front Page (72) Inventor Isamu Sato 2-9-13 Nakameguro, Meguro-ku, Tokyo Stanley Electric Co., Ltd.
Claims (2)
ＳｉＯ2／Ｖ2Ｏ5重量比で1.5〜3.5の範囲に均一に分散
した耐熱性黄色透明膜。1. A heat-resistant yellow transparent film in which fine vanadium pentoxide is uniformly dispersed in a range of 1.5 to 3.5 in terms of SiO 2 / V 2 O 5 weight ratio in silica.
溶液中に粒径0.2μm以下の五酸化バナジウム粉末が均一
に分散された黄色膜形成用組成物であって、五酸化バナ
ジウム粉末の含有量が、形成された膜中のＳｉＯ2／Ｖ2
Ｏ5 重量比で1.5〜3.5となる範囲であることを特徴とす
る耐熱性透明黄色膜形成用組成物。2. A yellow film-forming composition in which vanadium pentoxide powder having a particle size of 0.2 μm or less is uniformly dispersed in a solution of an alkyl silicate or silica sol, wherein the content of the vanadium pentoxide powder is formed. SiO 2 / V 2 in the film
A heat-resistant transparent yellow film-forming composition, wherein the O 5 weight ratio is in the range of 1.5 to 3.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33291291A JP3234264B2 (en) | 1991-11-22 | 1991-11-22 | Heat-resistant transparent yellow film and composition for forming the film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33291291A JP3234264B2 (en) | 1991-11-22 | 1991-11-22 | Heat-resistant transparent yellow film and composition for forming the film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0692623A true JPH0692623A (en) | 1994-04-05 |
| JP3234264B2 JP3234264B2 (en) | 2001-12-04 |
Family
ID=18260195
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33291291A Expired - Fee Related JP3234264B2 (en) | 1991-11-22 | 1991-11-22 | Heat-resistant transparent yellow film and composition for forming the film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3234264B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6300710B1 (en) | 1998-11-18 | 2001-10-09 | Ushiodenki Kabushiki Kaisha | Filament lamp for emission of yellow light |
| JP2005532978A (en) * | 2002-07-18 | 2005-11-04 | イーストマン コダック カンパニー | Method for producing aluminum silicate hybrid polymer and polymer obtained by the method |
-
1991
- 1991-11-22 JP JP33291291A patent/JP3234264B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6300710B1 (en) | 1998-11-18 | 2001-10-09 | Ushiodenki Kabushiki Kaisha | Filament lamp for emission of yellow light |
| JP2005532978A (en) * | 2002-07-18 | 2005-11-04 | イーストマン コダック カンパニー | Method for producing aluminum silicate hybrid polymer and polymer obtained by the method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3234264B2 (en) | 2001-12-04 |
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