JP7575991B2 - Multi-component glass molding and manufacturing method thereof - Google Patents
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本発明は、多成分ガラス成型品、およびその製造方法に関する。 The present invention relates to a multi-component glass molded product and a method for producing the same.
半導体製造工程では生産性向上のため、高密度プラズマ環境下でもプラズマ耐性に優れ、繰り返し使用においても腐食の少ない、プラズマ耐性を有する多成分ガラスが使用されている。多成分ガラスは、石英（ＳｉＯ2）にアルミナ（Ａｌ2Ｏ3）やイットリア（Ｙ2Ｏ3）などを添加したガラスである。多成分ガラスの製造方法としては、例えば、電気溶融法、プラズマ溶融法、酸水素炎溶融法などが知られている(特許文献１～５）。 In the semiconductor manufacturing process, in order to improve productivity, multi-component glass is used, which has excellent plasma resistance even in a high-density plasma environment and is less corroded even with repeated use. Multi-component glass is glass in which alumina (Al 2 O 3 ), yttria (Y 2 O 3 ), etc. are added to quartz (SiO 2 ). Known methods for manufacturing multi-component glass include, for example, the electric melting method, the plasma melting method, and the oxyhydrogen flame melting method (Patent Documents 1 to 5).
これらの方法では、ガラス原料粉末を溶融して、ガラスインゴット(塊)などが製造される。ガラスインゴット(塊)は、研削・研磨などの加工工程を経て所定の形状の多成分ガラス製品が提供される(特許文献１、２）。多成分ガラス製品の形状によっては、所定の形状の鋳型内で原料粉末を溶融し、所定の形状に成型した多成分ガラス製品が得られる（特許文献３、４）。 In these methods, glass raw material powder is melted to produce glass ingots (lumps), etc. The glass ingots (lumps) are processed by grinding, polishing, etc. to provide multi-component glass products of a predetermined shape (Patent Documents 1 and 2). Depending on the shape of the multi-component glass product, raw material powder is melted in a mold of a predetermined shape to obtain a multi-component glass product molded into the predetermined shape (Patent Documents 3 and 4).
特許文献１には、原料となる混合粉末をプラズマ火炎中で溶融してガラスインゴットを得る方法が開示されている。この方法では、運転中に混合粉末が供給管内で閉塞する等により運転が不安定となり、層状の気泡が発生し、あるいは炉内の煉瓦からの異物混入する課題が有る。この方法ではインゴットは製造できるが、例えば、リング形状のような複雑な形状の成型品を直接製造することは困難である。そのため、インゴットを成型品に加工する必要があり、加工において多量のガラスを研削・研磨することから、材料の歩留が低いという問題もある。 Patent Document 1 discloses a method for obtaining a glass ingot by melting a mixed powder of raw materials in a plasma flame. This method has problems such as unstable operation due to the mixed powder clogging the supply pipe during operation, the generation of layered bubbles, or the inclusion of foreign matter from the bricks in the furnace. Although this method can produce an ingot, it is difficult to directly produce molded products with complex shapes such as rings. Therefore, it is necessary to process the ingot into a molded product, and there is also the problem of low material yield because a large amount of glass is ground and polished during processing.
特許文献２には、酸水素バーナーを用いて原料粉末を溶解してガラスインゴットを得る方法が開示されている。この方法では、得られるガラスが微泡（～φ０．５）を含み、脱泡が困難である。また、特許文献１に記載の方法と同様に、リング形状のような複雑な形状の成型品の製造は困難なため、材料の歩留が低いという問題もある。 Patent Document 2 discloses a method of obtaining a glass ingot by melting raw material powder using an oxyhydrogen burner. With this method, the glass obtained contains fine bubbles (up to φ0.5), which are difficult to degas. Also, as with the method described in Patent Document 1, it is difficult to manufacture molded products with complex shapes such as ring shapes, which causes the problem of low material yield.
特許文献３および４には、カーボンモールド内に原料粉末を充填し、これを電気炉で減圧溶融して、モールドの内部形状に対応するガラスインゴット又は成型品を得る方法が開示されている。但し、リング形状のような複雑な形状の成型品の製造例の記載はない。特許文献３および４に記載の熱処理条件に従って追試をし、多成分ガラスを調製したところ、気泡：～φ０．３（局部的な集合気泡の残存）や異物：～φ１が残存することが、課題として明らかとなった。 Patent documents 3 and 4 disclose a method of filling a carbon mold with raw material powder, melting it under reduced pressure in an electric furnace, and obtaining a glass ingot or molded product that corresponds to the internal shape of the mold. However, there is no mention of an example of manufacturing a molded product with a complex shape such as a ring shape. When a multi-component glass was prepared by following up on the heat treatment conditions described in patent documents 3 and 4, it became clear that there were problems with bubbles of up to φ0.3 (residual localized aggregate bubbles) and foreign matter of up to φ1 remaining.
特許文献５には、製造方法の具体的な条件等の記載はない。 Patent document 5 does not include any specific manufacturing conditions.
まとめると、特許文献１および２に記載の製造方法は、品質、歩留の観点から適さない方法であった。特許文献３と４に記載の製造方法では、得られる多成分ガラスにおいて泡・異物が多く、品質に課題があった。 In summary, the manufacturing methods described in Patent Documents 1 and 2 were not suitable from the standpoint of quality and yield. The manufacturing methods described in Patent Documents 3 and 4 produced multi-component glass with many bubbles and foreign matter, posing quality issues.
最近、半導体製造装置に用いる耐プラズマ材料は、部品の高品位化、薄肉化を受けて、欠陥の少ない部材が要求されている。本発明は、こうした背景から耐プラズマガラス中の欠陥（泡・異物）を低減した多成分ガラス成型品を、製品歩留を向上しつつ、製造できる方法を提供することを目的とする。さらには、本発明は、従来にない程度に欠陥（泡・異物）を低減した、優れた耐プラズマ性を有する多成分ガラス成型品を提供することも目的とする。 Recently, plasma-resistant materials used in semiconductor manufacturing equipment are required to have fewer defects due to the trend toward higher quality and thinner parts. In light of this background, the present invention aims to provide a method for manufacturing multi-component glass molded products with reduced defects (bubbles and foreign matter) in the plasma-resistant glass while improving product yield. Furthermore, the present invention also aims to provide multi-component glass molded products with excellent plasma resistance and reduced defects (bubbles and foreign matter) to an unprecedented degree.
上記課題を解決する本発明は以下の通りである。
［１］
溶解部、混合部および成型部を有する成型装置を用いて多成分ガラス成型品を製造する方法であって、
（１）溶解部に多成分ガラスの原料混合粉を供給し、供給した原料混合粉を、原料混合粉組成の融点以上の温度で加熱して、原料混合粉の少なくとも一部が融解した融解前駆体を得る工程、
（２）得られた融解前駆体を、工程（１）より高い温度に加熱して融解液を得る工程、
（３）融解液を、混合部を介して成型部に供給する工程、及び
（４）成型部に供給した融解液を冷却して成型部の内部形状を反映した多成分ガラス成型品を得る工程を含み、
混合部は、融解液が流通することで混合される構造を有する、
前記製造方法。
［２］
多成分ガラスは、ケイ素（Ｓｉ）とアルミニウム（Ａｌ）と、周期表第２族元素、第３族元素及び第４族元素からなる群より選ばれる１種以上の元素（Ｍ）と、を含有する多成分ガラスである、［１］に記載の製造方法。
［３］
多成分ガラスは、ＳｉＯ2、Ａｌ2Ｏ3及びＹ2Ｏ3を含有する３成分ガラスであり、工程（１）における加熱温度は１３５０℃以上であり、工程（２）における加熱温度は、１６００℃以上である、［１］又は[２]に記載の製造方法。
[４]
工程（２）及び（３）における融解液の温度は、融解液の粘度ｌｏｇηが１．５Ｐａ・ｓである温度以上の温度である、［１］～[３]のいずれかに記載の製造方法。
[５]
工程（２）及び（３）における融解液の温度は、融解液の粘度ｌｏｇηが－０．５Ｐａ・ｓである温度以下の温度である、［１］～[４]のいずれかに記載の製造方法。
［６］
多成分ガラス成型品は、管状、柱状または平板状である、［１］～［５］のいずれかに記載の製造方法。
［７］
日本光学硝子規格における気泡および異物の等級はそれぞれ１等級または２等級である多成分ガラス成型品。
［８］
形状が管状、柱状または平板状である、［７］に記載の多成分ガラス成型品。
［９］
多成分ガラスは、アルミニウム（Ａｌ）と、周期表第２族元素、第３族元素及び第４族元素からなる群より選ばれる１種以上の元素（Ｍ）と、を含有する石英（ＳｉＯ2）ガラスである、［７］または［８］に記載の多成分ガラス成型品。
The present invention that solves the above problems is as follows.
[1]
A method for producing a multi-component glass molded product using a molding device having a melting section, a mixing section, and a molding section, comprising the steps of:
(1) a step of supplying a raw material mixture powder of a multi-component glass to a melting section and heating the supplied raw material mixture powder at a temperature equal to or higher than the melting point of the raw material mixture powder composition to obtain a molten precursor in which at least a part of the raw material mixture powder is melted;
(2) heating the obtained molten precursor to a temperature higher than that of the step (1) to obtain a molten liquid;
(3) supplying the molten liquid to a molding section through a mixing section; and (4) cooling the molten liquid supplied to the molding section to obtain a multi-component glass molded product that reflects the internal shape of the molding section,
The mixing section has a structure in which the molten liquid flows through the mixing section,
The manufacturing method.
[2]
The multi-component glass contains silicon (Si), aluminum (Al), and one or more elements (M) selected from the group consisting of elements of Groups 2, 3, and 4 of the periodic table.
[3]
The manufacturing method according to [1] or [2], wherein the multi-component glass is a three-component glass containing SiO 2 , Al 2 O 3 and Y 2 O 3 , the heating temperature in step (1) is 1350° C. or higher, and the heating temperature in step (2) is 1600° C. or higher.
[4]
The manufacturing method according to any one of [1] to [3], wherein the temperature of the molten liquid in steps (2) and (3) is equal to or higher than the temperature at which the viscosity log η of the molten liquid is 1.5 Pa s.
[5]
The manufacturing method according to any one of [1] to [4], wherein the temperature of the molten liquid in steps (2) and (3) is a temperature at which the viscosity log η of the molten liquid is −0.5 Pa s or lower.
[6]
The method according to any one of [1] to [5], wherein the multi-component glass molded product is tubular, columnar or flat.
[7]
A multi-component glass molding whose air bubbles and foreign matter are classified as grades 1 and 2 under the Japan Optical Glass Standards.
[8]
The multi-component glass molded product according to [7], which has a tubular, columnar or flat shape.
[9]
The multi-component glass is a silica (SiO 2 ) glass containing aluminum (Al) and one or more elements (M) selected from the group consisting of elements of Groups 2, 3, and 4 of the periodic table. The multi-component glass molded product according to [7] or [8].
本発明によれば、気泡及び異物がきわめて少ない優れた品質の多成分ガラス成型品を製造できる。この多成分ガラス成型品は、気泡及び異物がきわめて少ないことから耐プラズマ性に優れる。 The present invention makes it possible to produce high-quality multi-component glass molded products with very few air bubbles and foreign matter. These multi-component glass molded products have excellent plasma resistance because they contain very few air bubbles and foreign matter.
本発明においては、原料混合粉を融解及び成型する過程で各過程に適した３室構造（溶解室、混合室、成型室）を有する成型装置を用い、かつ溶解室における原料混合粉の融解条件を制御し、得られた融解液を混合室で混合して均質性を上げ、さらに、成型室に至るまでの融解液からの脱泡を促進することで、気泡及び異物がきわめて少ない優れた品質の多成分ガラス成型品を製造できる。 In the present invention, a molding device having a three-chamber structure (melting chamber, mixing chamber, molding chamber) suitable for each process is used in the process of melting and molding the raw material mixed powder, the melting conditions of the raw material mixed powder in the melting chamber are controlled, the resulting molten liquid is mixed in the mixing chamber to increase homogeneity, and further, degassing from the molten liquid before it reaches the molding chamber is promoted, thereby making it possible to manufacture high-quality multi-component glass molded products with very few air bubbles and foreign matter.
＜多成分ガラス成型品の製造方法＞
本発明の一の態様は、溶解部、混合部および成型部を有する成型装置を用いて多成分ガラス成型品を製造する方法に関する。本発明の製造方法は、
（１）溶解部に多成分ガラスの原料混合粉を供給し、供給した原料混合粉を、原料混合粉組成の融点以上の温度で加熱して、原料混合粉の少なくとも一部が融解した融解前駆体を得る工程、
（２）得られた融解前駆体を、工程（１）より高い温度に加熱して融解液を得る工程、
（３）得られた融解液を、混合部を介して成型部に供給する工程、及び
（４）成型部に供給した融解液を冷却して成型部の内部形状を反映した多成分ガラス成型品を得る工程を含む。
さらに上記混合部は、融解液が流通することで混合される構造を有する。
<Method of manufacturing multi-component glass molded products>
One aspect of the present invention relates to a method for producing a multi-component glass molded product using a molding device having a melting section, a mixing section, and a molding section. The manufacturing method of the present invention includes the steps of:
(1) a step of supplying a raw material mixture powder of a multi-component glass to a melting section and heating the supplied raw material mixture powder at a temperature equal to or higher than the melting point of the raw material mixture powder composition to obtain a molten precursor in which at least a part of the raw material mixture powder is melted;
(2) heating the obtained molten precursor to a temperature higher than that of the step (1) to obtain a molten liquid;
(3) supplying the obtained molten liquid to a molding section via a mixing section; and (4) cooling the molten liquid supplied to the molding section to obtain a multi-component glass molded product that reflects the internal shape of the molding section.
Furthermore, the mixing section has a structure in which the molten liquid flows through and is mixed.
本発明の製造方法に用いる成型装置は、溶解部、混合部および成型部を有する。この成型装置において、
溶解部は、供給した多成分ガラスの原料混合粉を溶解して融解液を得るための溶解室を有し、溶解室の内壁の少なくとも一部は剥離材で覆われており、
混合部は、融解液が流通することで混合される構造を有し、
成型部は、内部形状の少なくとも一部が多成分ガラス成型品の外部形状に相当する形状であり、かつ融解液を任意で脱泡し、次いで冷却して多成分ガラス成型品を得るための成型室を有し、成型室の内壁の少なくとも一部は剥離材で覆われている。
The molding apparatus used in the manufacturing method of the present invention has a melting section, a mixing section, and a molding section.
the melting section has a melting chamber for melting the supplied raw material mixed powder of the multi-component glass to obtain a molten liquid, and at least a part of the inner wall of the melting chamber is covered with a release material;
The mixing section has a structure in which the molten liquid flows through the mixing section,
The molding section has a molding chamber, at least a portion of whose internal shape corresponds to the external shape of the multi-component glass molded product, and in which the molten liquid is optionally degassed and then cooled to obtain the multi-component glass molded product, and at least a portion of the inner wall of the molding chamber is covered with a release material.
以下、成型装置について、説明し、次いで製造方法について説明する。
図１に成型装置の一態様を示す側面断面概略説明図である。図１に示す成型装置の平面形状は略円形である。図中、１は中実体、２は上蓋、３は外周筒体、４は剥離材、５は底板、６は貫通孔を有するプレート、７はプレートの間の距離を決定するスペーサーをそれぞれ示す。成型装置全体の外形は、外周筒体３及び底板５で構成され、その内側に剥離材４が設けられ、装置の内面を形成する。
The molding apparatus will now be described, followed by a description of the manufacturing method.
Fig. 1 is a schematic cross-sectional side view of one embodiment of a molding device. The planar shape of the molding device shown in Fig. 1 is approximately circular. In the figure, 1 denotes a solid body, 2 denotes an upper cover, 3 denotes an outer cylindrical body, 4 denotes a release material, 5 denotes a bottom plate, 6 denotes a plate having a through hole, and 7 denotes a spacer that determines the distance between the plates. The outer shape of the entire molding device is composed of an outer cylindrical body 3 and a bottom plate 5, and a release material 4 is provided inside thereof to form the inner surface of the device.
溶解部は、供給した多成分ガラスの原料混合粉を溶解するための溶解室１０を有する。溶解室１０は、円筒形であり、底面及び内側周面を有し、内側周面は、剥離材４で覆われており、剥離材４は少なくとも原料混合粉の少なくとも一部が融解した融解前駆体および融解液と接触する部分に設ける。底面は、後述する混合室２０を構成する最上層のプレート６ａの上面であり、この最上層のプレート６ａは貫通孔を有し、貫通孔は混合室２０に繋がる連絡孔となる。溶解室１０の上部は、原料を供給するために一部又は全部が開放口であり、図1の装置では、開放口に上蓋２を有する。溶解室１０は図示しない加熱装置及び温度センサーを備える。 The melting section has a melting chamber 10 for melting the supplied mixed powder of multi-component glass materials. The melting chamber 10 is cylindrical, has a bottom surface and an inner peripheral surface, and the inner peripheral surface is covered with a peeling material 4, which is provided at a portion where at least a portion of the mixed powder of materials comes into contact with the molten precursor and the molten liquid. The bottom surface is the upper surface of the top plate 6a constituting the mixing chamber 20 described later, and this top plate 6a has a through hole, which becomes a communication hole connected to the mixing chamber 20. The upper part of the melting chamber 10 is partially or entirely an opening for supplying the raw materials, and in the device of FIG. 1, the opening has an upper lid 2. The melting chamber 10 is equipped with a heating device and a temperature sensor, not shown.
混合部は、溶解部において原料混合粉が融解して得られた融解液が流通することで混合される構造を有する混合室２０を有する。混合室２０の内径は、溶解室１０の内径と実質的に同一であり、混合室２０の内側周面は、剥離材４で覆われ、最上層のプレート６ａにより、溶解室１０と混合室２０とが区画されている。混合室２０内には、単一または複数の貫通孔を有するプレートを縦方向に２層以上有する。図１の装置では、６ａ、６ｂ及び６ｃの３層のプレートが設けられ、隣り合うプレートの間にはスペーサー７がそれぞれ設けられ、プレートの間の距離を決定する。一のプレートに設けられた貫通孔は、隣接する他のプレートに設けられた貫通孔と実質的に対向しない位置関係で設置される。そうすることで、混合室２０内を融解液が流通ときに混合が促進される。混合室２０は、図示しない加熱装置及び温度センサーを備えることができる。図２、３に、貫通孔を有するプレートの平面形状の例を示す。 The mixing section has a mixing chamber 20 having a structure in which the raw material mixed powder is melted in the melting section and the molten liquid obtained flows through it. The inner diameter of the mixing chamber 20 is substantially the same as the inner diameter of the melting chamber 10, and the inner peripheral surface of the mixing chamber 20 is covered with a peeling material 4, and the melting chamber 10 and the mixing chamber 20 are partitioned by the top plate 6a. The mixing chamber 20 has two or more layers of plates having a single or multiple through holes arranged vertically. In the device of FIG. 1, three layers of plates 6a, 6b, and 6c are provided, and spacers 7 are provided between adjacent plates to determine the distance between the plates. The through holes provided in one plate are installed in a positional relationship that does not substantially face the through holes provided in the other adjacent plates. This promotes mixing when the molten liquid flows through the mixing chamber 20. The mixing chamber 20 can be equipped with a heating device and a temperature sensor (not shown). Figures 2 and 3 show examples of the planar shape of a plate having a through hole.
図２に示すプレートは、直径ｒ１の略円板状であり、外周縁に長さＬ１、深さＬ２の切欠きを１又は２以上有する。直径ｒ１は、混合室２０の内径に相当する。この切欠きがプレートの貫通孔を形成する。一のプレートに４箇所の切欠きを設ける場合、切欠きの長さＬ１がプレートの全外周縁長の１／８以下であれば、複数のプレートを例えば、４５°毎にローテーションして複数層設けることで、一のプレートに設けられた貫通孔は、隣接する他のプレートに設けられた貫通孔と実質的に対向しない位置となる。各プレートの切欠きの位置関係をこのように設定した混合室２０を、融解液が流通することで、融解液の混合は促進される。所謂、スタティックミキサーの構造となる。切欠きの形状、寸法及び設置数は、融解液の粘度や混合室２０内に設置するプレートの枚数、混合により得られる融解液の均質性等を考慮して適宜決定できる。１つのプレートにおける切欠きの設置数は、例えば、１～１０、好ましくは２～８、より好ましくは３～６である。 The plate shown in FIG. 2 is approximately disc-shaped with a diameter r1, and has one or more notches with a length L1 and a depth L2 on the outer periphery. The diameter r1 corresponds to the inner diameter of the mixing chamber 20. The notches form the through holes of the plate. When four notches are provided in one plate, if the length L1 of the notch is 1/8 or less of the total outer periphery length of the plate, the through holes provided in one plate are positioned so as not to substantially face the through holes provided in the other adjacent plates by rotating the multiple plates, for example, every 45°. The mixing of the molten liquid is promoted by the flow of the molten liquid through the mixing chamber 20 in which the positional relationship of the notches of each plate is set in this way. This is the structure of a so-called static mixer. The shape, dimensions and number of the notches can be appropriately determined taking into consideration the viscosity of the molten liquid, the number of plates to be installed in the mixing chamber 20, the homogeneity of the molten liquid obtained by mixing, etc. The number of notches in one plate is, for example, 1 to 10, preferably 2 to 8, and more preferably 3 to 6.
図３に示すプレートは、略円板状であり、略円板状の直径は、混合室２０の内径に相当する。外周縁近くに直径ｒ２の略円形の貫通孔を１又は２以上有する。図３のプレートは、４個の貫通孔を有し、上下に隣接するプレート６ａ、６ｂ、６ｃは、４５°にずらしてローテーションしてあり、平面図には最上層のプレート６ａの４つの貫通孔を実線で示し、その下のプレート６ｂの貫通孔を破線で示す。各プレートと貫通孔との位置関係をＡ－Ｃ断面及びＢ－Ｄ断面に示す。各プレートに設ける貫通孔の直径ｒ２を調整することで、一のプレートに設けられた貫通孔は、隣接する他のプレートに設けられた貫通孔と実質的に対向しない位置に設けることができる。これらのプレートを設けた混合室２０を溶解した多成分ガラスが流通することで、融解液の混合は促進される。貫通孔の個数、貫通孔の寸法及び設置数は、融解液の粘度や混合室２０内に設置するプレートの枚数、混合により得られる融解液の均質性等を考慮して適宜決定できる。１つのプレートにおける貫通孔の設置数は、例えば、１～１０、好ましくは２～８、より好ましくは３～６である。 The plate shown in FIG. 3 is substantially circular, and the diameter of the substantially circular shape corresponds to the inner diameter of the mixing chamber 20. It has one or more substantially circular through holes with a diameter r2 near the outer periphery. The plate in FIG. 3 has four through holes, and the upper and lower adjacent plates 6a, 6b, and 6c are rotated at a 45° angle. In the plan view, the four through holes of the uppermost plate 6a are shown in solid lines, and the through holes of the plate 6b below are shown in dashed lines. The positional relationship between each plate and the through holes is shown in the A-C and B-D cross sections. By adjusting the diameter r2 of the through holes provided in each plate, the through holes provided in one plate can be provided at a position that does not substantially face the through holes provided in the other adjacent plates. The flow of the melted multi-component glass through the mixing chamber 20 provided with these plates promotes the mixing of the molten liquid. The number of through holes, the size of the through holes, and the number of holes to be installed can be determined appropriately taking into consideration the viscosity of the molten liquid, the number of plates to be installed in the mixing chamber 20, the homogeneity of the molten liquid obtained by mixing, etc. The number of through holes installed in one plate is, for example, 1 to 10, preferably 2 to 8, and more preferably 3 to 6.
成型部は、目的とする成型品の形状に応じた内部形状を有する成型室３０を有し、図１に示す成型室３０は、管状(パイプ状)又はシリンダー状の成型品を成型するように管状成型品の中空を形成するための中実体を有する内部形状を有する。底面、外周面及び内周面を有する。底面、外周面及び内周面は、剥離材４で覆われる。内周面を覆う剥離材は、中実体１の外周面に固定される。成型室３０の上部は、少なくとも一部が開放口であり、混合室２０に繋がる。図２に示す混合部用のプレートの最下層のプレートが有する貫通孔（切欠き）が、成型室３０の上部の開放口と対向し、貫通孔（切欠き）から成型室３０内に混合室２０で混合された融解液を流入させる構造を有する。図３に示す混合部用のプレートの場合も、最下層のプレート６ｃが有する貫通孔が、成型室３０の上部の開放口と対向し、貫通孔から成型室３０内に混合室２０で混合された融解液を流入させる構造を有する。成型室３０は図示しない加熱装置及び温度センサーを備える。 The molding section has a molding chamber 30 having an internal shape corresponding to the shape of the desired molded product, and the molding chamber 30 shown in FIG. 1 has an internal shape with a solid body for forming a hollow of a tubular molded product so as to mold a tubular (pipe-shaped) or cylindrical molded product. It has a bottom surface, an outer peripheral surface, and an inner peripheral surface. The bottom surface, outer peripheral surface, and inner peripheral surface are covered with a release material 4. The release material covering the inner peripheral surface is fixed to the outer peripheral surface of the solid body 1. At least a part of the upper part of the molding chamber 30 is an open port, which is connected to the mixing chamber 20. The through hole (notch) of the bottom plate of the mixing section plate shown in FIG. 2 faces the open port at the top of the molding chamber 30, and has a structure that allows the molten liquid mixed in the mixing chamber 20 to flow into the molding chamber 30 from the through hole (notch). In the case of the plate for the mixing section shown in FIG. 3, the through hole of the bottom plate 6c faces the upper opening of the molding chamber 30, and is structured so that the molten liquid mixed in the mixing chamber 20 flows into the molding chamber 30 through the through hole. The molding chamber 30 is equipped with a heating device and a temperature sensor, not shown.
図１に示す成型装置は、溶解部、混合部及び成型部を一体とした成型装置であるが、これらは別の構造とすることも可能である。 The molding device shown in Figure 1 is a molding device that integrates the melting section, mixing section, and molding section, but these can also be of different structures.
以下、製造方法について説明する。
工程（１）
（１）溶解部に多成分ガラスの原料混合粉を供給し、供給した原料混合粉を、原料混合粉組成の融点以上の温度で加熱して、原料混合粉の少なくとも一部が融解した融解前駆体を得る。
The manufacturing method will be described below.
Step (1)
(1) A raw material mixture powder of a multi-component glass is supplied to a melting section, and the supplied raw material mixture powder is heated to a temperature equal to or higher than the melting point of the raw material mixture powder composition to obtain a molten precursor in which at least a portion of the raw material mixture powder is melted.
多成分ガラスは、特に制限はなく、例えば、ケイ素（Ｓｉ）とアルミニウム（Ａｌ）と、ＩＵＰＡＣ形式での周期表第２族元素（アルカリ土類金属）、第３族元素（希土類）及び第４族元素（チタン族）からなる群より選ばれる１種以上の元素（Ｍ）と、を含有する多成分石英（ＳｉＯ2）ガラスであることができる。周期表第２族元素（アルカリ土類金属）は、例えば、Ｍｇ、Ｃａ、Ｓｒ、Ｂａであり、第３族元素（希土類）は、Ｓｃ、Ｙ、Ｌａなどであり、第４族元素（チタン族）は、Ｔｉ、Ｚｒ、Ｈｆなどである。多成分ガラスの原料は、所望の組成を有する混合粉であることができ、上記元素の酸化物、炭酸塩、硝酸塩、塩化物などであることができ、粉末原料は既存の原料をそのまま使用できる。混合粉末の組成についても特に制限はない。但し、純度の高い多成分ガラスを得るという観点からは、酸化物を用いることが好ましく、不純物含有量の低い酸化物原料を用いることが特に好ましい。粉末原料の粒子径には特に制限はないが、例えば、０．１～１０００μｍの範囲の任意の粒子径の粉末を用いることができる。 The multi-component glass is not particularly limited, and may be, for example, a multi-component quartz (SiO 2 ) glass containing silicon (Si), aluminum (Al), and one or more elements (M) selected from the group consisting of elements of Group 2 (alkaline earth metals), Group 3 (rare earth), and Group 4 (titanium group) of the periodic table in the IUPAC format. The elements of Group 2 (alkaline earth metals) of the periodic table are, for example, Mg, Ca, Sr, and Ba, the elements of Group 3 (rare earth) are Sc, Y, La, and the like, and the elements of Group 4 (titanium group) are Ti, Zr, and Hf, and the like. The raw material of the multi-component glass may be a mixed powder having a desired composition, and may be an oxide, carbonate, nitrate, chloride, or the like of the above elements, and the powder raw material may be an existing raw material as it is. There is also no particular limit to the composition of the mixed powder. However, from the viewpoint of obtaining a multi-component glass with high purity, it is preferable to use an oxide, and it is particularly preferable to use an oxide raw material with a low impurity content. There is no particular restriction on the particle size of the powder raw material, but for example, powders having any particle size in the range of 0.1 to 1000 μm can be used.
多成分ガラスの具体例は、ＳｉＯ2、Ａｌ2Ｏ3及びＹ2Ｏ3を含有する３成分ガラスであることができる。これら酸化物の混合粉を多成分ガラス原料として用いることができ、各酸化物の融点は、ＳｉＯ2が１７１０℃、Ａｌ2Ｏ3が２０７２℃、Ｙ2Ｏ3が２４２５℃である。但し、上記３成分ガラスの融点は、組成により約１３００～１５００℃であり、かつ透明なガラスが得られる組成領域がある（日本金属学誌 第６７巻 第１号（２００３）４０－４６、Ｆｉｇ．２参照）。本発明では、多成分ガラスの成型品を得るために上記透明なガラスが得られる組成領域であり、かつ比較的融点の低い組成領域を選択し、その組成領域にある混合粉を、原料混合粉組成の融点以上の温度で加熱して原料混合粉の少なくとも一部が融解した融解前駆体を得る。この加熱により、原料粉末の少なくとも一部は反応してガラス又はガラス前駆体である融解前駆体を形成する。但し、原料粉末の反応が急激に進行して、ガラス中に異物や泡が多量に生じることを抑制する目的で、加熱温度は、融解前駆体の粘度ｌｏｇηが１．５Ｐａ・ｓとなる温度未満の温度とすることが好ましい。融解前駆体の粘度ｌｏｇηが１．５Ｐａ・ｓとなる温度は、原料粉末の組成により決まる。上記３成分ガラスの場合、この粘度範囲を示す温度の目安は、１３５０～１６００℃、好ましくは１４００～１５５０℃の範囲である。この温度域における加熱により、原料混合粉は反応をしつつ、粘度ｌｏｇηが１．５Ｐａ・ｓより大きい値を示す融解前駆体を得ることができる。融解液を得る前に、この融解前駆体を形成する工程を経ることが、溶解室内の剥離材とガラス原料との不要な反応による泡の発生を抑制するという観点から好ましい。 A specific example of the multi-component glass may be a three-component glass containing SiO 2 , Al 2 O 3 and Y 2 O 3. A mixed powder of these oxides may be used as a raw material for the multi-component glass, and the melting points of the oxides are 1710°C for SiO 2 , 2072°C for Al 2 O 3 and 2425°C for Y 2 O 3 . However, the melting points of the above three-component glasses are about 1300 to 1500°C depending on the composition, and there is a composition region in which transparent glass can be obtained (see Japanese Journal of Metal Science and Technology, Vol. 67, No. 1 (2003) 40-46, Fig. 2). In the present invention, in order to obtain a molded product of a multi-component glass, a composition region in which the above-mentioned transparent glass can be obtained and which has a relatively low melting point is selected, and the mixed powder in that composition region is heated at a temperature equal to or higher than the melting point of the raw material mixed powder composition to obtain a molten precursor in which at least a part of the raw material mixed powder is melted. By this heating, at least a part of the raw material powder reacts to form a molten precursor which is a glass or a glass precursor. However, in order to prevent the reaction of the raw material powder from proceeding too quickly and causing a large amount of foreign matter or bubbles in the glass, the heating temperature is preferably set to a temperature below the temperature at which the viscosity log η of the molten precursor becomes 1.5 Pa·s. The temperature at which the viscosity log η of the molten precursor becomes 1.5 Pa·s is determined by the composition of the raw material powder. In the case of the above three-component glass, the temperature range showing this viscosity range is 1350 to 1600°C, preferably 1400 to 1550°C. By heating in this temperature range, the raw material mixed powder reacts and a molten precursor showing a viscosity log η greater than 1.5 Pa·s can be obtained. It is preferable to go through the process of forming this molten precursor before obtaining the molten liquid from the viewpoint of preventing the generation of bubbles due to unnecessary reactions between the peeling material and the glass raw material in the melting chamber.
工程（１）においては、原料粉同士が反応して、互いに結合し、さらには溶融すると考えられ、その際に粒子間に気体を巻き込み、後の工程で融解液中における泡となる。加熱温度を低めに設定することで脱泡すべき泡の量を減少させて、泡品質を向上するという観点から、工程（１）の反応時の泡の混入を抑制することが好ましい。 In step (1), the raw material powders react with each other, bond with each other, and are thought to melt. In the process, gas is trapped between the particles, which becomes bubbles in the molten liquid in a later step. From the viewpoint of reducing the amount of bubbles to be degassed and improving the quality of the bubbles, it is preferable to suppress the inclusion of bubbles during the reaction in step (1).
工程（２）
工程（１）で得られた融解前駆体を、工程（１）より高い温度に加熱して融解液を得る。加熱温度は、融解液の粘度ｌｏｇηが１．５Ｐａ・ｓである温度以上の温度とすることが、融解液からの脱泡促進と、次の工程における混合部を介しての成型部への供給が容易になるという観点から好ましい。加熱温度は、融解液の粘度ｌｏｇηが０．５Ｐａ・ｓである温度以上であることがより好ましい。溶解液の粘度が低すぎると流下の速度が増し次の工程での混合が困難になるため、加熱温度は、粘度は－０．５Ｐａ・ｓとなる温度以下が好ましい。粘度が－０．１Ｐａ・ｓとなる温度以下がより好ましい。上記３成分ガラスの場合、加熱温度は、例えば、１５５０～１８００℃、好ましくは１６００～１７５０℃の範囲とすることができる。
Step (2)
The molten precursor obtained in step (1) is heated to a temperature higher than that in step (1) to obtain a molten liquid. The heating temperature is preferably set to a temperature at which the viscosity log η of the molten liquid is 1.5 Pa·s or higher, from the viewpoint of promoting degassing from the molten liquid and facilitating supply to the molding part through the mixing part in the next step. The heating temperature is more preferably set to a temperature at which the viscosity log η of the molten liquid is 0.5 Pa·s or higher. If the viscosity of the melt is too low, the flow rate increases and mixing in the next step becomes difficult, so the heating temperature is preferably set to a temperature at which the viscosity is −0.5 Pa·s or lower. More preferably, the viscosity is set to −0.1 Pa·s or lower. In the case of the above three-component glass, the heating temperature can be, for example, in the range of 1550 to 1800° C., preferably 1600 to 1750° C.
工程（３）
融解液を、混合部を介して成型部に供給する。混合部は、融解液が流通することで混合される構造、具体的には上記のように所謂、スタティックミキサーの機能を有し、混合部を流通することで、混合され、均一化する。融解液の温度は、工程（２）と同一であることができ、融解液の混合と均一化が促進されるという観点及び融解液からの脱泡が容易であるという観点からは、融解液の粘度ｌｏｇηが１．５Ｐａ・ｓである温度以上の温度範囲であることが好ましい。加熱温度は、融解液の粘度ｌｏｇηが０．５Ｐａ・ｓである温度以上であることがより好ましい。溶解部から混合部を介して成型部に融解液が供給されるに要する時間は、融解液の量、混合部の構造されに融解液の粘度などにより変化する。融解液の供給の間に、融解液からの脱泡が進み泡品質を向上することができるので、所望の泡品質を考慮して供給完了までの時間を決定することもできる。
Step (3)
The melt is supplied to the molding section through the mixing section. The mixing section has a structure in which the melt flows and is mixed, specifically, has the function of a so-called static mixer as described above, and is mixed and homogenized by flowing through the mixing section. The temperature of the melt can be the same as that of the step (2), and from the viewpoint of promoting the mixing and homogenization of the melt and from the viewpoint of facilitating defoaming from the melt, it is preferable that the temperature range is equal to or higher than the temperature at which the viscosity log η of the melt is 1.5 Pa·s. It is more preferable that the heating temperature is equal to or higher than the temperature at which the viscosity log η of the melt is 0.5 Pa·s. The time required for the melt to be supplied from the dissolving section to the molding section through the mixing section varies depending on the amount of the melt, the structure of the mixing section, the viscosity of the melt, and the like. During the supply of the melt, defoaming from the melt progresses and the foam quality can be improved, so the time until the supply is completed can also be determined in consideration of the desired foam quality.
成型部に供給された融解液は、十分に溶解され、原料粉末に比べて反応性は低くなっているため、高い温度であっても成型室の内壁を構成する剥離材との反応は抑制でき、泡の減少及び異物混入の抑制が可能である。 The molten liquid supplied to the molding section is fully dissolved and has a lower reactivity than the raw material powder, so even at high temperatures it is possible to suppress reaction with the release material that makes up the inner wall of the molding chamber, reducing bubbles and preventing the inclusion of foreign matter.
工程（４）
成型部に供給した融解液を冷却して成型部の内部形状を反映した多成分ガラス成型品を得る。融解液の冷却は、成型装置を、冷却速度を制御しつつ放冷するなどして実施できる。工程（２）及び（３）において融解液からの脱泡は進み、成型部に供給された融解液からも順次脱泡が進むことが効率的な脱泡という観点からは好ましい。
Step (4)
The molten liquid supplied to the molding section is cooled to obtain a multi-component glass molded product that reflects the internal shape of the molding section. The molten liquid can be cooled by, for example, allowing the molding device to cool while controlling the cooling rate. In steps (2) and (3), degassing from the molten liquid proceeds, and it is preferable from the viewpoint of efficient degassing that degassing proceed successively from the molten liquid supplied to the molding section.
本発明の装置を用いるガラス成型品の製造は、バッチ式で行うことも連続式で行うこともできる。連続式の場合、同一のガラス組成で、異なる形状及び寸法の成型部を用いることで、異なる形状の成型品を連続的に製造することも可能である。 The production of glass molded products using the apparatus of the present invention can be carried out in a batch or continuous manner. In the case of a continuous process, it is possible to continuously produce molded products of different shapes by using molding parts of different shapes and dimensions with the same glass composition.
本発明の装置及び方法を用いることで、日本光学硝子規格における気泡および異物の等級はそれぞれ１等級または２等級である多成分ガラス成型品を得ることができる。本発明は、日本光学硝子規格における気泡および異物の等級はそれぞれ１等級または２等級である多成分ガラス成型品を包含する。本発明の多成分ガラス成型品は、形状が管状、柱状または平板状であることができる。多成分ガラス成型品を構成する多成分ガラスは、例えば、ケイ素（Ｓｉ）とアルミニウム（Ａｌ）に加えて、周期表第２族元素、第３族元素及び第４族元素からなる群より選ばれる１種以上の元素（Ｍ）を含有する多成分ガラスであることができる。多成分ガラス成型品を構成する多成分ガラスは、ＳｉＯ2、Ａｌ2Ｏ3及びＹ2Ｏ3を含有する３成分ガラスであることができる。ＳｉＯ2、Ａｌ2Ｏ3及びＹ2Ｏ3を含有する３成分ガラスは、例えば、ＳｉＯ2 ２０～６０ｗｔ％、Ａｌ2Ｏ3 １０～５０ｗｔ％、Ｙ2Ｏ3 ２０～６０ｗｔ％の組成範囲のガラスであることができ、好ましくはＳｉＯ2：２７．５～４３．３ ｗｔ％、Ａｌ2Ｏ3：１８．３～３２．５ ｗｔ％、Ｙ2Ｏ3：２５～４５ ｗｔ％の組成範囲である(参考文献：日本金属学誌 第６７巻 第１号（２００３）４０－４６）。 By using the device and method of the present invention, it is possible to obtain a multi-component glass molded product having a grade of 1 or 2 for bubbles and foreign matter according to the Japan Optical Glass Standards. The present invention includes a multi-component glass molded product having a grade of 1 or 2 for bubbles and foreign matter according to the Japan Optical Glass Standards. The multi-component glass molded product of the present invention can be tubular, columnar, or flat. The multi-component glass constituting the multi-component glass molded product can be, for example, a multi-component glass containing, in addition to silicon (Si) and aluminum (Al), one or more elements (M) selected from the group consisting of Group 2 elements, Group 3 elements, and Group 4 elements of the periodic table. The multi-component glass constituting the multi-component glass molded product can be a three-component glass containing SiO 2 , Al 2 O 3 , and Y 2 O 3 . The three-component glass containing SiO 2 , Al 2 O 3 and Y 2 O 3 may be, for example, a glass having a composition range of SiO 2 20-60 wt %, Al 2 O 3 10-50 wt %, and Y 2 O 3 20-60 wt %, and preferably has a composition range of SiO 2 : 27.5-43.3 wt %, Al 2 O 3 : 18.3-32.5 wt %, and Y 2 O 3 : 25-45 wt % (Reference: Journal of the Japan Society of Metals, Vol. 67, No. 1 (2003) 40-46).
以下、本発明を実施例に基づいて更に詳細に説明する。但し、実施例は本発明の例示であって、本発明は実施例に限定される意図ではない。 The present invention will be described in more detail below with reference to examples. However, the examples are merely illustrative of the present invention, and the present invention is not intended to be limited to the examples.
１）混合粉末の調製
以下の原料を用いて以下に示す方法で混合粉末を調製した。
（ｉ）原料粉末
・ＳｉＯ2：シリカ粉末（純度９９．９％以上）、
・Ａｌ2Ｏ3：アルミナ粉末（純度９９．９％以上）、
・Ｙ2Ｏ3：イットリア粉末（純度９９．９％以上）、
（ｉｉ）調合
ＳｉＯ2：４０ ｗｔ％、Ａｌ2Ｏ3：３０ ｗｔ％、Ｙ2Ｏ3：３０ ｗｔ％となるように上記原料粉末を、ウレタン製ボールを入れた１０Ｌのポリエチレン製混合ポットに０．５～３ｋｇを供給し、回転台で混合する。
1) Preparation of Mixed Powder A mixed powder was prepared using the following raw materials by the method described below.
(i) Raw material powder: SiO2 : silica powder (purity 99.9% or more);
Al2O3 : Alumina powder (purity 99.9% or more),
Y2O3 : yttria powder ( purity 99.9% or more),
(ii) Preparation 0.5 to 3 kg of the above raw material powders are fed into a 10 L polyethylene mixing pot containing a urethane ball and mixed on a rotating table so that the composition is SiO 2 : 40 wt %, Al 2 O 3 : 30 wt %, and Y 2 O 3 : 30 wt %.
２）成型型及び粉末の混合粉末の融解
実施例１
図１に示す成型装置を使用して表２に示すサイズのバイプ状の多成分ガラス成型品を調製した。溶解室に上記１）で調製した混合粉末０．６７ｋｇを充填し、高温炉内で１４００℃、４時間溶解した。次いで、温度を１６５０℃に上げ、２時間経過させて融解液とし、融解液は、混合室を経由して成型室に自重で流下した。その際の溶解室、混合室及び成型室の温度は１６５０℃とし、融解液中の残存気泡を脱泡させた。成型室への融解液の流下に３０分間を要し、その後、成型装置全体を放冷して、室温になった後に成型室から成型品を取り出した。
2) Molding mold and powder mixture Melting Example 1
Using the molding apparatus shown in FIG. 1, pipe-shaped multi-component glass molded products of the size shown in Table 2 were prepared. 0.67 kg of the mixed powder prepared in 1) above was filled into the melting chamber and melted in a high-temperature furnace at 1400°C for 4 hours. The temperature was then raised to 1650°C and left for 2 hours to form a molten liquid, which then flowed down by its own weight through the mixing chamber into the molding chamber. The temperatures of the melting chamber, mixing chamber and molding chamber at this time were set to 1650°C, and residual bubbles in the molten liquid were degassed. It took 30 minutes for the molten liquid to flow down into the molding chamber, after which the entire molding apparatus was allowed to cool to room temperature and the molded product was removed from the molding chamber.
尚、上記組成の混合粉末を加熱して得られる融解前駆体および融解液の粘性は、１，４５０℃：ｌｏｇη＝１．２５Ｐａ・ｓ、１，５５０℃：ｌｏｇη＝－０．１５Ｐａ・ｓ、１６５０℃：ｌｏｇη＝－０．８Ｐａ・ｓであり、１，４５０℃以上で流動できる条件である。上記実施例では、加熱温度１，４００℃として溶解室内で原料粉末を融解前駆体に変化させる。この時の融解前駆体の粘性はｌｏｇη＝－０．１５Ｐａ・ｓである。その後１，６５０℃まで昇温してｌｏｇη＝－０．５Ｐａ・ｓである融解液とした後に溶解室から混合室を経て成型室に融解液を移動させた。上記粘度を有する融解液は、溶解室から混合室を経て成型室に至る間および成型室においての脱泡が進んだ。 The viscosity of the molten precursor and molten liquid obtained by heating the mixed powder of the above composition is 1,450°C: log η = 1.25 Pa·s, 1,550°C: log η = -0.15 Pa·s, and 1650°C: log η = -0.8 Pa·s, which is a condition that allows flow at 1,450°C or higher. In the above example, the raw material powder is changed into a molten precursor in the melting chamber at a heating temperature of 1,400°C. The viscosity of the molten precursor at this time is log η = -0.15 Pa·s. The temperature is then raised to 1,650°C to produce a molten liquid with log η = -0.5 Pa·s, and the molten liquid is then moved from the melting chamber through the mixing chamber to the molding chamber. The molten liquid with the above viscosity degassed while passing from the melting chamber through the mixing chamber to the molding chamber and in the molding chamber.
実施例２
混合粉末量は３６ｋｇとし、温度を１６５０℃に上げた後に３時間経過させた以外は、実施例１と同様にして成型品を調製した。
Example 2
A molded product was prepared in the same manner as in Example 1, except that the amount of mixed powder was 36 kg and 3 hours were allowed to pass after the temperature was raised to 1650°C.
比較例１
図１に示す成型装置の成型室に相当する形状の、図４に記載の従来技術の成型型を用いて、表２に記載の実施例１と同様のサイズのバイプ状の多成分ガラス成型品を調製した。成型型は１室構造で、粉末の融解、脱泡、成型を同じ室で行う。上記１）で調製した混合粉末６７０ｇを充填し、１４００℃で４時間溶解した。次いで、温度を１６５０℃に上げ、２時間経過させ、融液中の残存気泡を脱泡さ、その後、成型装置全体を放冷して、室温になった後に成型室から成型品を取り出した。
Comparative Example 1
A pipe-shaped multi-component glass molded product of the same size as in Example 1 listed in Table 2 was prepared using a conventional mold shown in FIG. 4, which has a shape corresponding to the molding chamber of the molding device shown in FIG. 1. The mold has a single chamber structure, and the melting, degassing, and molding of the powder are performed in the same chamber. 670 g of the mixed powder prepared in 1) above was filled and melted at 1400°C for 4 hours. The temperature was then raised to 1650°C and left for 2 hours to degas the remaining bubbles in the melt, after which the entire molding device was allowed to cool to room temperature and the molded product was removed from the molding chamber.
３）成型品の品質
〈評価方法〉
成型型から取り出した成型品は、成型品外表面を研削もしくは輪切りし、切断面を研削する。加工した評価サンプルは研削面であるため、屈折率が同じ疑似液を塗布し、日本光学硝子工業会規格の光学ガラスの泡の測定方法と光学ガラスの異物の測定方法に準じて観察し、等級評価した。
表１に日本光学硝子工業規格を示す。
3) Quality of molded products (assessment method)
The molded product removed from the mold is ground or sliced, and the cut surface is ground. Since the processed evaluation sample is the ground surface, a simulated liquid with the same refractive index is applied to it, and it is observed and graded according to the Japan Optical Glass Industry Association standard methods for measuring bubbles in optical glass and for measuring foreign matter in optical glass.
Table 1 shows the Japan Optical Glass Industry Standards.
〈成型品の品質〉
実施例１及び２、並びに比較例１で得られた成型品の品質を表２に示す。
実施例１及び２の成型品内の泡及び異物は日本光学硝子規格等級：１等級であった。従来技術の成型型を用いた比較例１の成型品は、泡及び異物に関する品質は３等級及び４等級であり、満足できる品質ではなかった。
<Quality of molded products>
The qualities of the molded products obtained in Examples 1 and 2 and Comparative Example 1 are shown in Table 2.
The bubbles and foreign matter in the molded products of Examples 1 and 2 were classified as Grade 1 according to the Japan Optical Glass Standards. The molded product of Comparative Example 1, which used a molding die of the prior art, was classified as Grade 3 and Grade 4 in terms of quality in terms of bubbles and foreign matter, which were not of satisfactory quality.
多成分ガラス成型品の製造に関する分野に有用である。 Useful in the field of manufacturing multi-component glass moldings.
Claims (7)
（１）溶解部に多成分ガラスの原料混合粉を供給し、供給した原料混合粉を、原料混合粉組成の融点以上の温度で加熱して、原料混合粉の少なくとも一部が融解した融解前駆体を得る工程、
（２）得られた融解前駆体を、工程（１）より高い温度に加熱して融解液を得る工程、
（３）融解液を、混合部を介して成型部に供給する工程、及び
（４）成型部に供給した融解液を冷却して成型部の内部形状を反映した多成分ガラス成型品を得る工程を含み、
前記成型装置は、平面形状が略円形であり、外形が外周筒体及び底板で構成され、外周筒体及び底板で構成される装置内に、溶解部となる溶解室、混合部となる混合室及び成形部となる成形室を有し、混合室の内径は、溶解室の内径と実質的に同一であり、
溶解室は、上部の一部又は全部が開放口であり、前記外周筒体の内側周面及び底面を有し、底面は、混合室を構成する最上層のプレートの上面であり、この最上層のプレートは混合室に繋がる貫通孔を有し、
混合部は、単一または複数の貫通孔を有するプレートを流れ方向に２層以上有し、隣り合うプレートの間にはスペーサーがそれぞれ設けられ、一のプレートに設けられた貫通孔は、隣接する他のプレートに設けられた貫通孔と実質的に対向しない位置関係で設置される混合室を有し、かつ融解液が前記プレートの貫通孔を流通することで混合される構造を有し、
工程（１）の加熱、工程（２）の加熱及び工程（４）の冷却は、成形装置を一体として操作する、
多成分ガラス成型品の製造方法。 A method for producing a multi-component glass molded product using a molding device having a melting section, a mixing section, and a molding section, comprising the steps of:
(1) a step of supplying a raw material mixture powder of a multi-component glass to a melting section and heating the supplied raw material mixture powder at a temperature equal to or higher than the melting point of the raw material mixture powder composition to obtain a molten precursor in which at least a part of the raw material mixture powder is melted;
(2) heating the obtained molten precursor to a temperature higher than that of the step (1) to obtain a molten liquid;
(3) supplying the molten liquid to a molding section through a mixing section; and (4) cooling the molten liquid supplied to the molding section to obtain a multi-component glass molded product that reflects the internal shape of the molding section,
the molding device has a substantially circular planar shape and an outer shape formed of an outer cylindrical body and a bottom plate, the molding device formed of the outer cylindrical body and the bottom plate has a melting chamber serving as a melting section, a mixing chamber serving as a mixing section, and a molding chamber serving as a molding section, the inner diameter of the mixing chamber being substantially the same as the inner diameter of the melting chamber,
the melting chamber has an upper portion, part or all of which is an open port, and has an inner peripheral surface and a bottom surface of the outer peripheral cylinder, the bottom surface being the upper surface of a top plate constituting the mixing chamber, the top plate having a through hole communicating with the mixing chamber;
the mixing section has two or more layers of plates each having a single or a plurality of through holes arranged in the flow direction, a spacer is provided between each pair of adjacent plates, the through hole in one plate has a mixing chamber disposed in a positional relationship such that the through hole is not substantially opposed to the through hole in the other adjacent plate, and the molten liquid is mixed by flowing through the through holes in the plates ;
The heating in step (1), the heating in step (2), and the cooling in step (4) are performed in an integrated molding apparatus .
A method for manufacturing multi-component glass moldings.
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