JP2008050262A - Method for clarifying alkali-free glass - Google Patents
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本発明は歪点の高い無アルカリガラスの清澄方法に関する。 The present invention relates to a method for refining alkali-free glass having a high strain point.
従来、各種ディスプレイ用基板ガラス、特に表面に金属ないし酸化物の薄膜等を形成させるものでは、以下に示す特性が要求されてきた。
(1)アルカリ金属酸化物を含有していると、アルカリ金属イオンが薄膜中に拡散して、膜特性を劣化させてしまうため、実質的にアルカリ金属イオンを含まないこと。
(2)薄膜形成工程で高温にさらされるため、ガラスの変形およびガラスの構造安定化に伴う収縮(熱収縮)を最小限に抑えるため、高い歪点を有すること。
Conventionally, various display substrate glasses, particularly those in which a thin film of metal or oxide is formed on the surface, have been required to have the following characteristics.
(1) If an alkali metal oxide is contained, the alkali metal ions diffuse into the thin film and deteriorate the film characteristics, so that the alkali metal ions are not substantially contained.
(2) Since it is exposed to a high temperature in the thin film formation process, it has a high strain point in order to minimize the shrinkage (thermal shrinkage) associated with glass deformation and glass structural stabilization.
(3)半導体形成に用いられる各種薬品に対して充分な化学耐久性を有すること。特にSiOx やSiNx のエッチングのためのバッファードフッ酸(フッ酸+フッ化アンモニウム;BHF)、およびITOのエッチングに用いられる塩酸を含有する薬液、金属電極のエッチングに用いられる各種の酸(硝酸、硫酸等)、レジスト剥離液のアルカリに対して耐久性があること。
(4)内部および表面に欠点(泡、脈理、インクルージョン、ピット、キズ等)をもたないこと。
(3) Sufficient chemical durability against various chemicals used for semiconductor formation. In particular, buffered hydrofluoric acid (hydrofluoric acid + ammonium fluoride; BHF) for etching SiO x and SiN x , and chemicals containing hydrochloric acid used for etching ITO, various acids used for etching metal electrodes ( Nitric acid, sulfuric acid, etc.) and resist stripper alkali.
(4) No defects (bubbles, striae, inclusions, pits, scratches, etc.) inside and on the surface.
電子用途の基板ガラスでは上記(4)の品質に対する要求は厳しい。したがって、特に泡を効率的に除く目的で、従来の基板ガラスではヒ素やアンチモンを1〜2重量%添加してガラスの熔解し、清澄を行うことが多かった。ヒ素やアンチモンは高温粘性の高いガラスの清澄剤として知られている。 In the case of substrate glass for electronic use, the demand for the quality of (4) is severe. Therefore, for the purpose of efficiently removing bubbles, conventional substrate glasses often add 1 to 2% by weight of arsenic or antimony to melt and clarify the glass. Arsenic and antimony are known as high-viscosity glass fining agents.
しかし、ヒ素やアンチモン、特にヒ素は、環境に悪影響を与える元素であるため、ガラスのリサイクルに支障が生じるうえ、ガラスの製造工場や処理工場内でのガラスの取り扱いに注意が必要であり、かつエッチング廃液の無害化処理にも多大の設備が必要であった。 However, since arsenic and antimony, especially arsenic, are elements that adversely affect the environment, glass recycling is hindered, and attention must be paid to the handling of glass in glass manufacturing plants and processing plants, and A large amount of equipment was also required for the detoxification treatment of the etching waste liquid.
本発明の目的は、歪点の高い無アルカリガラスの熔解において、ヒ素やアンチモンを使用しないか、使用量をごく少量としても清澄が可能なガラスの熔解時の清澄方法を提供することにある。 It is an object of the present invention to provide a clarification method at the time of melting glass that can be clarified even if the amount of the arsenic or antimony is not used or the amount used is very small in melting of alkali-free glass having a high strain point.
本発明は、歪点が640℃以上でAs2 O3 含有量が0.5重量%以下の無アルカリガラスを熔解時に清澄する方法であって、1.5重量%以下のSb2 O3 、5.0重量%以下のSO3 、2.0重量%以下のFe2 O3 および5.0重量%以下のSnO2 からなる群から選ばれる1種以上の有効量と、5.0重量%以下のClおよび5.0重量%以下のFからなる群から選ばれる1種以上の有効量とを含有せしめて熔解、清澄することを特徴とする清澄方法を提供する。 The present invention is a method for refining an alkali-free glass having a strain point of 640 ° C. or higher and an As 2 O 3 content of 0.5% by weight or less during melting, comprising 1.5% by weight or less of Sb 2 O 3 , One or more effective amounts selected from the group consisting of 5.0 wt% or less SO 3 , 2.0 wt% or less Fe 2 O 3 and 5.0 wt% or less SnO 2 , and 5.0 wt% There is provided a clarification method comprising melting and clarifying by containing at least one effective amount selected from the group consisting of the following Cl and 5.0 wt% or less F.
本発明は、本発明者らが特定の清澄剤の組み合わせを用いることにより、清澄効果を高め、歪点の高い無アルカリガラスの熔解において、ヒ素やアンチモンを使用しないか、使用量を少量としても清澄できることを知見したことに基づく。 The present invention improves the clarification effect by using a combination of specific clarifiers by the present inventors, and does not use arsenic or antimony in the melting of alkali-free glass having a high strain point, even if the amount used is small. Based on finding out that it can be clarified.
本発明によるガラスは、人体および地球環境を悪化させずに、高品質なガラス基板(ディスプレイ用基板、フォトマスク基板、TFTタイプのディスプレイ基板等)、およびその製造方法として好適である。 The glass according to the present invention is suitable as a high-quality glass substrate (display substrate, photomask substrate, TFT type display substrate, etc.) and a manufacturing method thereof without deteriorating the human body and the global environment.
本発明では、Sb2 O3 、SO3 、Fe2 O3 およびSnO2 のいずれか1つ以上、ならびにFおよびClのいずれか1つ以上が有効量添加されることが必須である。有効量は無アルカリガラスの組成にも依存するが、一般的には、それぞれ合量で0.01重量%以上含有されれば効果がある。これらの清澄剤が併用されることにより、飛躍的に清澄効果が高まる。なお、添加量をあまり多くしても効果が飽和する一方、ガラスの特性に影響を与えるおそれがあるため、それぞれ合量で5.0重量%以下、好ましくは2.0重量%以下、とすることが実用的である。 In the present invention, it is essential to add an effective amount of any one or more of Sb 2 O 3 , SO 3 , Fe 2 O 3 and SnO 2 , and any one or more of F and Cl. The effective amount depends on the composition of the alkali-free glass, but in general, it is effective if the total amount is 0.01% by weight or more. By using these fining agents in combination, the fining effect is dramatically increased. In addition, although the effect is saturated even if the addition amount is excessively large, there is a possibility that the properties of the glass may be affected. Therefore, the total amount is 5.0% by weight or less, preferably 2.0% by weight or less. It is practical.
このうち、Sb2 O3 は高温粘性の大きいガラスの清澄剤として知られており、同様の機能を持つAs2 O3 よりも環境への悪影響が少ない。その添加量は、環境への悪影響を最小限とするため、1.5重量以下とする。1.0重量%以下とすることが好ましく、特に好ましくは不純物の程度を超えて実質的に含有されない。 Among these, Sb 2 O 3 is known as a glass refining agent having a high temperature viscosity and has less adverse effects on the environment than As 2 O 3 having the same function. The amount added is 1.5 wt. Or less in order to minimize adverse effects on the environment. The content is preferably 1.0% by weight or less, particularly preferably not substantially contained beyond the level of impurities.
SO3 は原料に熱を加えていく際に多量の泡を発生し、かつ、泡を大きくする成分であり、建築用にしばしば用いられるソーダライムシリケートガラスの清澄剤として用いられることが多い。SO3 源は無アルカリであるかぎり、どのような塩の形で加えてもよいが、通常はアルカリ土類の硫酸塩として加える。0.01重量%以上添加することにより、清澄効果が得られる。添加量が多すぎると、泡の発生が過剰となり原料へ添加する意味がないため、実用上は5.0重量%以下、好ましくは2.0重量%以下、とされる。 SO 3 is a component that generates a large amount of foam when heat is applied to the raw material and enlarges the foam, and is often used as a fining agent for soda lime silicate glass often used for construction. The SO 3 source may be added in any salt form as long as it is alkali-free, but is usually added as an alkaline earth sulfate. A clarification effect can be obtained by adding 0.01% by weight or more. If the amount added is too large, the generation of bubbles becomes excessive and there is no point in adding to the raw material, so that it is practically 5.0% by weight or less, preferably 2.0% by weight or less.
Fe2 O3 は原料に熱を加えていく際にFe2 O3 →Fe2 O+O2 となって酸素泡を発生する成分である。0.01重量%以上添加することにより、清澄効果が得られる。添加量をあまり多くしても効果が飽和する一方、ガラスの着色が著しくなるため、2.0重量%以下、好ましくは1.0重量%以下、とする。 Fe 2 O 3 is a component that generates oxygen bubbles as Fe 2 O 3 → Fe 2 O + O 2 when heat is applied to the raw material. A clarification effect can be obtained by adding 0.01% by weight or more. Even if the addition amount is too large, the effect is saturated, but the coloring of the glass becomes remarkable, so that it is 2.0% by weight or less, preferably 1.0% by weight or less.
SnO2 は原料に熱を加えていく際にSnO2 →SnO+1/2・O2 となって酸素泡を発生する成分である。0.01重量%以上添加することにより、清澄効果が得られる。添加量をあまり多くしても効果が飽和する一方、ガラスの特性に影響を与えるおそれがあるため、5.0重量%以下、好ましくは2.0重量%以下、とする。 SnO 2 is a component that generates oxygen bubbles as SnO 2 → SnO + 1/2 · O 2 when heat is applied to the raw material. A clarification effect can be obtained by adding 0.01% by weight or more. Even if the addition amount is too large, the effect is saturated, but there is a possibility of affecting the properties of the glass. Therefore, it is 5.0% by weight or less, preferably 2.0% by weight or less.
一方、FやClも、原料に熱を加えていく際に多量の泡を発生し、かつ、泡を大きくする成分であるが、上記Sb2 O3 、SO3 、Fe2 O3 およびSnO2 のいずれか1つ以上と併用することにより、清澄効果が飛躍的に向上する。これらは、通常、アルカリ土類のフッ化物や塩化物として加えうる。それぞれ0.01重量%以上添加することにより、清澄効果が得られる。添加量をあまり多くしても効果が飽和する一方、ガラスの特性(特に歪点低下)に影響を与えるおそれがあるため、5.0重量%以下、好ましくは2.0重量%以下とする。 On the other hand, F and Cl are components that generate a large amount of bubbles and increase the bubbles when heat is applied to the raw material, but the above-mentioned Sb 2 O 3 , SO 3 , Fe 2 O 3 and SnO 2. By using together with any one or more of the above, the clarification effect is dramatically improved. These can usually be added as alkaline earth fluorides or chlorides. A clarification effect is obtained by adding 0.01% by weight or more of each. Even if the addition amount is too large, the effect is saturated, but there is a possibility of affecting the characteristics of the glass (especially lowering of the strain point), so it is 5.0% by weight or less, preferably 2.0% by weight or less.
本発明はアルカリ金属酸化物を実質的に含有しない無アルカリガラスで、歪点が640℃以上のものを対象とする。かかるガラスは、清澄可能な温度が高温域にあるため、ソーダライムシリケートガラスのように通常の芒硝による清澄ができないと考えられており、ヒ素による清澄が行われていた。 The present invention is a non-alkali glass that does not substantially contain an alkali metal oxide and has a strain point of 640 ° C. or higher. Such glass has a clarification temperature in a high temperature range, and it is considered that clarification with ordinary sodium sulfate cannot be performed unlike soda lime silicate glass, and clarification with arsenic has been performed.
具体的には、重量表示で実質的に以下のような組成が例示できる。
SiO2 40〜80%、
Al2 O3 0〜35%、
B2 O3 0〜25%、
MgO 0〜30%、
CaO 0〜30%、
SrO 0〜30%、
BaO 0〜30%、
MgO+CaO+SrO+BaO 1〜50%。
Specifically, the following compositions can be exemplified substantially in terms of weight.
SiO 2 40~80%,
Al 2 O 3 0-35%,
B 2 O 3 0-25%,
MgO 0-30%,
CaO 0-30%,
SrO 0-30%,
BaO 0-30%,
MgO + CaO + SrO + BaO 1-50%.
特に、以下のような2種類の組成は歪点が高いため、高温粘性が大きく、本発明が効果的に適用できる。すなわち、重量表示で実質的に、
SiO2 55〜65%、
Al2 O3 10〜18%、
B2 O3 0〜 3%、
MgO 0〜 3%、
CaO 8〜15%、
SrO 8〜15%、
BaO 0〜 2%、
MgO+CaO+SrO+BaO 10〜35%、
または、
SiO2 58.4〜65.0%、
Al2 O3 15.3〜22.0%、
B2 O3 5.0〜12.0%、
MgO 0〜 6.0%、
CaO 0〜 7.0%、
SrO 4.0〜12.0%、
BaO 0〜 2.0%、
MgO+CaO+SrO+BaO
9.0〜18.0%、
となるものである。
In particular, the following two types of compositions have a high strain point and thus have a high temperature viscosity, and the present invention can be effectively applied. That is, in weight display,
SiO 2 55~65%,
Al 2 O 3 10-18%,
B 2 O 3 0 to 3%,
MgO 0 to 3%,
CaO 8-15%,
SrO 8-15%,
BaO 0-2%,
MgO + CaO + SrO + BaO 10-35%,
Or
SiO 2 58.4~65.0%,
Al 2 O 3 15.3 to 22.0%,
B 2 O 3 5.0 to 12.0%,
MgO 0 to 6.0%,
CaO 0 to 7.0%,
SrO 4.0-12.0%,
BaO 0-2.0%,
MgO + CaO + SrO + BaO
9.0 to 18.0%,
It will be.
本発明のガラスは、例えば次のような方法で製造できる。
通常使用される各成分の原料を目標成分になるように調合し、本発明の所定の清澄剤を添加したのち、これを熔解炉に連続的に投入し、1500〜1600℃に加熱して熔融する。この熔融ガラスを1200〜1500℃に保持することにより、泡ぬき(清澄)し、フロート法等により所定の板厚に成形し、徐冷後切断する。清澄時に減圧を併用してもよい。
The glass of the present invention can be produced, for example, by the following method.
The raw materials of each component that is normally used are prepared so as to become target components, and after adding the predetermined fining agent of the present invention, it is continuously charged into a melting furnace and heated to 1500 to 1600 ° C. for melting. To do. By holding this molten glass at 1200 to 1500 ° C., bubbles are removed (clarified), formed into a predetermined plate thickness by a float method or the like, and then cooled and cut. You may use decompression together at the time of clarification.
このようにして、製造されたガラスは、ガラス中に重量表示で
As2 O3 0〜0.5%、
Sb2 O3 0〜1.5%、
SO3 0〜5.0%、
Fe2 O3 0〜2.0%、
SnO2 0〜5.0%、
Sb2 O3 +SO3 +Fe2 O3 +SnO2
0.01〜5.0%、
Cl 0〜5.0%、
F 0〜5.0%、
Cl+F 0.01〜5.0%、
を含有する無アルカリガラスである。ヒ素、アンチモンは実質的に含有されないことが好ましい。
Thus, the manufactured glass is As 2 O 3 0-0.5% by weight display in glass,
Sb 2 O 3 0-1.5%,
SO 3 0-5.0%,
Fe 2 O 3 0-2.0%,
SnO 2 0-5.0%,
Sb 2 O 3 + SO 3 + Fe 2 O 3 + SnO 2
0.01-5.0%,
Cl 0-5.0%,
F 0-5.0%,
Cl + F 0.01-5.0%,
Is an alkali-free glass. It is preferable that arsenic and antimony are not substantially contained.
表に本発明の実施例を示す。
SiO2 、Al2 O3 、B2 O3 、MgO、CaO、SrOおよびBaOは工業用原料を用いて合計で100重量部となるように調合し、Sb2 O3 、SO3 、Cl、F、Fe2 O3 およびSnO2 (清澄剤)はこれに上乗せする形で加えた。
Examples of the present invention are shown in the table.
SiO 2 , Al 2 O 3 , B 2 O 3 , MgO, CaO, SrO and BaO are prepared using industrial raw materials so that the total amount becomes 100 parts by weight, and Sb 2 O 3 , SO 3 , Cl, F Fe 2 O 3 and SnO 2 (fining agent) were added on top of this.
表中に示した「泡数(1)」は調合原料バッチ(500g)を白金坩堝に入れ、1600℃で1時間熔解、徐冷後のガラス表面から1cm下から2cm下までの間にある泡の数(個/g)を示す。また、「泡数(2)」には調合原料バッチ(500g)を白金坩堝にいれ1600℃で30分熔解後、通常のスクリュー状のスターラを用いて20rpmで撹拌しながら20分熔融、徐冷後のガラス表面から1cm下から2cm下までの間にある泡の数(個/g)を示す。 “Number of bubbles (1)” shown in the table is a bubble between 1 cm to 2 cm below the glass surface after putting the blended raw material batch (500 g) into a platinum crucible and melting at 1600 ° C. for 1 hour. Number (pieces / g). In addition, in “Number of bubbles (2)”, the raw material batch (500 g) was placed in a platinum crucible and melted at 1600 ° C. for 30 minutes, and then melted and slowly cooled for 20 minutes while stirring at 20 rpm using a normal screw-shaped stirrer. The number of bubbles (pieces / g) between 1 cm below and 2 cm below the subsequent glass surface is shown.
表にはガラスの50〜350℃での平均の熱膨張係数と歪点と耐塩酸性も示す。例1〜19は実施例、例20〜38は比較例である。特に例1〜8と例24〜27とを比較することにより、清澄剤の併用の効果がわかる。 The table also shows the average thermal expansion coefficient, strain point, and hydrochloric acid resistance of glass at 50 to 350 ° C. Examples 1 to 19 are examples, and examples 20 to 38 are comparative examples. In particular, by comparing Examples 1 to 8 and Examples 24 to 27, the effect of the combined use of the clarifying agent can be seen.
実施例のガラスは泡数(1)に示すように熔融初期に泡の残りと、泡数(2))に示すように撹拌したときの泡の熔け残り、撹拌リボイル(再沸)泡がいずれも少なく、また、ガラスの均一性も良く、高品質なガラスの製造に適当であることがわかる。
また、これらの清澄剤は熱膨張係数、歪点、耐塩酸性に影響を与えず、好ましい清澄剤であるといえる。
In the glass of the example, the remaining foam at the initial stage of melting as indicated by the number of bubbles (1), the unmelted bubbles when stirred as indicated by the number of bubbles (2)), and the stirred reboiling (re-boiling) bubbles In addition, it is understood that the glass has good uniformity and is suitable for the production of high-quality glass.
These fining agents do not affect the thermal expansion coefficient, strain point, and hydrochloric acid resistance, and can be said to be preferable fining agents.
また、SO3 、Cl、Fの量は添加量で示しているが、これらガラスを熔融する間に一部揮散してしまうため残存量はこれより少なくなる。この残存量はガラス組成に依存する。例えば、例3では、0.2%のF、0.2%のCl、0.05%のSO3 などの残存がある。 Moreover, although the amount of SO 3 , Cl, and F is shown as an addition amount, the remaining amount is smaller than this because some of the glass is volatilized during melting. This remaining amount depends on the glass composition. For example, in Example 3, there are residuals of 0.2% F, 0.2% Cl, 0.05% SO 3 and the like.
Claims (5)
SiO2 58.4〜65.0%、
Al2 O3 15.3〜22.0%、
B2 O3 5.0〜12.0%、
MgO 0〜 6.0%、
CaO 0〜 7.0%、
SrO 4.0〜12.0%、
BaO 0〜 2.0%、
MgO+CaO+SrO+BaO 9.0〜18.0%。 A method of clarifying alkali-free glass having a strain point of 640 ° C. or higher, containing the following components by weight, and having an As 2 O 3 content of 0.5% by weight or less at the time of melting: 1.5% by weight The total amount of at least one selected from the group consisting of the following Sb 2 O 3 , 5.0 wt% or less SO 3 , 2.0 wt% or less Fe 2 O 3 and 5.0 wt% or less SnO 2 0.01 to 5.0% by weight and SnO 2 is 0.01 to 5.0% by weight, one selected from the group consisting of Cl of 5.0% by weight or less and F of 5.0% by weight or less A non-alkali glass clarification method comprising melting and refining by adding 0.01 to 5.0% by weight of the total amount as described above.
SiO 2 58.4~65.0%,
Al 2 O 3 15.3 to 22.0%,
B 2 O 3 5.0 to 12.0%,
MgO 0 to 6.0%,
CaO 0 to 7.0%,
SrO 4.0-12.0%,
BaO 0-2.0%,
MgO + CaO + SrO + BaO 9.0-18.0%.
SiO2 58.4〜65.0%、
Al2 O3 15.3〜22.0%、
B2 O3 5.0〜12.0%、
MgO 0〜 6.0%、
CaO 0〜 7.0%、
SrO 4.0〜12.0%、
BaO 0〜 2.0%、
MgO+CaO+SrO+BaO 9.0〜18.0%、
As2 O3 0〜0.5%、
Sb2 O3 0〜1.5%、
SO3 0〜5.0%、
Fe2 O3 0〜2.0%、
SnO2 0.01〜5.0%、
Sb2 O3 +SO3 +Fe2 O3 +SnO2
0.01〜5.0%、
Cl 0〜5.0%、
F 0〜5.0%、
Cl+F 0.01〜5.0%、
を含有する無アルカリガラス。 In the glass, 58.4 to 65.0% SiO 2 by weight,
Al 2 O 3 15.3 to 22.0%,
B 2 O 3 5.0 to 12.0%,
MgO 0 to 6.0%,
CaO 0 to 7.0%,
SrO 4.0-12.0%,
BaO 0-2.0%,
MgO + CaO + SrO + BaO 9.0-18.0%,
As 2 O 3 0-0.5%,
Sb 2 O 3 0-1.5%,
SO 3 0-5.0%,
Fe 2 O 3 0-2.0%,
SnO 2 0.01-5.0%,
Sb 2 O 3 + SO 3 + Fe 2 O 3 + SnO 2
0.01-5.0%,
Cl 0-5.0%,
F 0-5.0%,
Cl + F 0.01-5.0%,
Alkali-free glass containing
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JP2007268221A JP2008050262A (en) | 2007-10-15 | 2007-10-15 | Method for clarifying alkali-free glass |
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JP2007268221A JP2008050262A (en) | 2007-10-15 | 2007-10-15 | Method for clarifying alkali-free glass |
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JP13008897A Division JP4739468B2 (en) | 1997-05-20 | 1997-05-20 | Alkali-free glass and its clarification method |
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Cited By (3)
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WO2013136949A1 (en) * | 2012-03-14 | 2013-09-19 | 旭硝子株式会社 | Float glass plate and method of manufacture thereof |
JP2015006973A (en) * | 2013-05-31 | 2015-01-15 | 日本電気硝子株式会社 | Composition for glass fiber, glass fiber and manufacturing method of glass fiber |
JP2015024946A (en) * | 2013-06-21 | 2015-02-05 | 日本電気硝子株式会社 | Composition for glass fiber, glass fiber and method of producing glass fiber |
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WO2013136949A1 (en) * | 2012-03-14 | 2013-09-19 | 旭硝子株式会社 | Float glass plate and method of manufacture thereof |
CN104169230A (en) * | 2012-03-14 | 2014-11-26 | 旭硝子株式会社 | Float glass plate and method of manufacture thereof |
JPWO2013136949A1 (en) * | 2012-03-14 | 2015-08-03 | 旭硝子株式会社 | Float glass plate and manufacturing method thereof |
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JP2015006973A (en) * | 2013-05-31 | 2015-01-15 | 日本電気硝子株式会社 | Composition for glass fiber, glass fiber and manufacturing method of glass fiber |
JP2015024946A (en) * | 2013-06-21 | 2015-02-05 | 日本電気硝子株式会社 | Composition for glass fiber, glass fiber and method of producing glass fiber |
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