JP3234264B2 - Heat-resistant transparent yellow film and composition for forming the film - Google Patents
Heat-resistant transparent yellow film and composition for forming the filmInfo
- Publication number
- JP3234264B2 JP3234264B2 JP33291291A JP33291291A JP3234264B2 JP 3234264 B2 JP3234264 B2 JP 3234264B2 JP 33291291 A JP33291291 A JP 33291291A JP 33291291 A JP33291291 A JP 33291291A JP 3234264 B2 JP3234264 B2 JP 3234264B2
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- Japan
- Prior art keywords
- film
- composition
- heat
- forming
- vanadium pentoxide
- 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.)
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- Silicon Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Surface Treatment Of Glass (AREA)
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 applied to 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 or alarm lamps for lighting vehicles and ships. The present invention 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 As a method of forming a colored film, there are conventionally known an electrostatic coating method, a sputtering method, a CVD method, a coating liquid coating method and the like. Have their own problems. In the electrostatic coating method, it is difficult to control to optimize the particle size of the coating material, and the particles are easily aggregated, so that light scattering is likely to occur and transparency is poor.
In addition, the sputtering method and the CVD method require expensive equipment and have poor productivity. On the other hand, the coating method has good productivity, can easily form a uniform film, and can easily control the composition. However, the conventionally known yellow 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 are optionally contained in a system of iron oxide and titanium oxide. (JP-A-54-
No. 101821), those in which 0.1 μm or less of zinc oxide or the like is dispersed in a solvent or a binder (Japanese Patent Application Laid-Open Nos.
No. 6) is known, but these films have poor heat resistance at high temperatures of about 500 ° C. The present inventor, various materials for heat-resistant glass used in 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
And so on. However, each of them has a small extinction coefficient and is not effective as a colored thin film, or has a disadvantage that it deteriorates immediately in a high-temperature environment, and is insufficient as a heat-resistant colored film.
【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 An object of the present invention is to provide a highly heat-resistant transparent yellow film which solves the above-mentioned problems and a composition for forming the film. The present inventor has continued to study a high heat-resistant yellow transparent film and a composition for forming the film, and as a result, the silicon-vanadium-based oxide forms a yellow-based transparent film having more excellent heat resistance than the conventional film. I found something 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: A solution means the configuration of the invention], in the silica, uniformly dispersed heat resistance yellow transparent in the range of 1.5 to 3.5 with a fine vanadium pentoxide SiO 2 / V 2 O 5 weight ratio A membrane is provided. Furthermore, according to the present invention, a composition for forming a yellow film 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 a silica sol, and the content of the vanadium pentoxide powder is: A composition for forming a heat-resistant transparent yellow film, wherein the weight ratio of SiO 2 / V 2 O 5 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 It 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 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 is undesirably reduced. Vanadium pentoxide is preferably fine particles having a particle size of 0.2 μm or less. When the particle size is larger than 0.2 μm, the transparency of the coating film is reduced. On the other hand, when the particle diameter of vanadium pentoxide is 0.2 μm or less, a wavelength of about 500 nm or less can be efficiently absorbed, and at a wavelength longer than that, a film having excellent transparency can be obtained.
【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 of the present invention can be prepared by a solution method (sol-gel method), CV
It can be formed by a usual method such as a D method or a sputtering method. As an example of the CVD method, tetraethoxyorthosilane is placed in a sealed container containing a heat-resistant transparent substrate.
(TEOS) and triethoxyvanadyl raw material gas
The coating is prepared in a weight ratio of iO 2 / V 2 O 5 in the range of 1.5 to 3.5, and the above-mentioned coating is grown on the surface of the transparent substrate by vapor phase. When the sputtering method is used, the weight ratio of SiO 2 / V 2 O 5 is 1.5 to
The sputtering target described in 3.5 is prepared, and the coating can be formed on the surface of the heat-resistant transparent substrate using the sputtering target.
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 an alkyl silicate or a silica sol, and the content of the vanadium pentoxide powder is formed. SiO 2 /
A composition for forming a heat-resistant transparent yellow film, wherein the weight ratio of V 2 O 5 is 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。[0007] As a silicon dioxide source of the composition solution used in the solution method, an alkyl silicate or a 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, tetraethoxyorthosilane (TEOS), tetramethylorthosilane (TMOS), tetrapropylorthosilane
(TPOS), tetrabutylorthosilane (TBOS), methylethoxysilane (MTES), dimethyldiethoxysilane, or a simple substance or a mixture thereof is used. When an alkyl silicate is used, for example, the alkyl silicate is dissolved in a solvent such as an alcohol and then partially hydrolyzed by adding dilute hydrochloric acid, and the concentration of the solid (SiO 2 ) formed is adjusted with an alcohol or the like so as to have an appropriate concentration. It is preferable to use after adjusting.
【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。[0008] The amount of the fine vanadium pentoxide powder mixed with the composition solution is in the range where the weight ratio of SiO 2 / V 2 O 5 in the formed film is 1.5 to 3.5. The method for uniformly dispersing the 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 addition, when mixing, it is preferable to sufficiently disperse the vanadium pentoxide powder in the composition solution over a sufficient time. If the dispersion is insufficient, the vanadium pentoxide grains easily grow in a high-temperature environment of 500 ° C. or more, causing clouding and devitrification of the film in a short time, failing to obtain a heat-resistant effect. The composition solution of the present invention is applied to one or both sides of a transparent substrate such as heat-resistant glass, heated, and thermally decomposed to obtain a highly heat-resistant yellow transparent body. The thickness of the coating film, the coating method and the heating method may be performed according to a conventional method. The formed film is a transparent film having a yellow color tone, and its 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 -based coating of the present invention is a yellow film having high heat resistance and excellent transparency. It has high heat resistance and is suitable for use at high temperatures. Further, the composition for forming a film can be easily applied to a transparent substrate such as a halogen lamp for lighting or an alarm lamp and heated to easily form a transparent yellow film having high heat resistance.
【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 5.00 g of tetraethoxyorthosilane (TEOS) was dissolved in isopropanol, and diluted hydrochloric acid was added for partial hydrolysis.
The concentration was adjusted with isopropanol so that the weight of the solid (SiO 2 ) became 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 therein, mixed well, and stirred with a ball mill for 100 hours 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, dried by heating, and the chromaticity (x, y) of the XYZ color system =
(0.498, 0.448), Y = 85.1, a yellow colored transparent body was obtained. As shown in FIG. 1, the Y value of this colored product when kept at a high temperature of 700 ° C. did not substantially change, 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 After dissolving 5.00 g of tetraethoxyorthosilane (TEOS) in isopropanol and adding dilute hydrochloric acid to partially hydrolyze,
The concentration was adjusted with isopropanol so that the weight of the solid (SiO 2 ) became 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 therein, mixed well, and 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, dried by heating, and the chromaticity (x, y) of the XYZ color system =
(0.504, 0.449), Y = 84.8, a yellow colored transparent body was obtained. The heat resistance when this colored body was held at a high temperature of 700 ° C. was the same as in 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 a 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 was (0.496,
0.4538), Y = 79.4 to obtain a yellow colored transparent body. FIG. 2 shows a change in Y value when the colored body is held at a high temperature of 700 ° C. As shown in the figure, the colored body of this example has a film turbidity in a short time,
Devitrification occurred and heat resistance was poor. This is considered to be because the dispersibility of vanadium pentoxide was lower than that in Example 1 and grain growth easily occurred.
【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 graph showing a change over time of a Y value when the colored body of the present invention obtained in Example 1 is maintained 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 diagram showing a change over 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 (56)参考文献 特開 昭63−48358（ＪＰ，Ａ) 特開 平２−265976（ＪＰ，Ａ) 特開 昭56−78445（ＪＰ，Ａ) 特開 平２−157137（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C03C 1/00 - 23/00 C01B 33/12 - 33/44 ──────────────────────────────────────────────────続 き Continuation of the front page (72) Inventor Isamu Sato 2-9-13 Nakameguro, Meguro-ku, Tokyo Inside Stanley Electric Co., Ltd. (56) References JP-A-63-48358 (JP, A) JP-A-63-48358 Hei 2-265976 (JP, A) JP-A-56-78445 (JP, A) JP-A 2-157137 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C03C 1 / 00-23/00 C01B 33/12-33/44
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 silica in a weight ratio of 1.5 to 3.5 in a SiO 2 / V 2 O 5 weight ratio.
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 composition for forming a yellow film in which a 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 composition for forming a heat-resistant transparent yellow film, wherein the weight ratio of O 5 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 JPH0692623A (en) | 1994-04-05 |
| JP3234264B2 true 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) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3506618B2 (en) | 1998-11-18 | 2004-03-15 | ウシオ電機株式会社 | Incandescent light bulb for yellow light emission |
| FR2842515B1 (en) * | 2002-07-18 | 2004-10-01 | Eastman Kodak Co | PROCESS FOR PREPARING A HYBRID ALUMINOSILICATE POLYMER AND POLYMER OBTAINED BY THIS PROCESS |
-
1991
- 1991-11-22 JP JP33291291A patent/JP3234264B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0692623A (en) | 1994-04-05 |
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