JP2011207719A - Synthetic amorphous silica powder and method for producing the same - Google Patents
Synthetic amorphous silica powder and method for producing the same Download PDFInfo
- Publication number
- JP2011207719A JP2011207719A JP2010078940A JP2010078940A JP2011207719A JP 2011207719 A JP2011207719 A JP 2011207719A JP 2010078940 A JP2010078940 A JP 2010078940A JP 2010078940 A JP2010078940 A JP 2010078940A JP 2011207719 A JP2011207719 A JP 2011207719A
- Authority
- JP
- Japan
- Prior art keywords
- glass powder
- silica glass
- synthetic silica
- producing
- spherical
- 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.)
- Withdrawn
Links
Landscapes
- Glass Melting And Manufacturing (AREA)
- Silicon Compounds (AREA)
Abstract
【課題】球状の不純物が少ない合成シリカガラス粉末を経済的に製造することができる方法、およびこの方法によって製造した球状の合成シリカガラス粉末を提供する。
【解決手段】合成したシリカ質のゲルをスプレー乾燥して球状化し、この球状乾燥粒子を焼成してガラス化することを特徴とする合成シリカガラス粉末の製造方法であり、好ましくは、球状乾燥粒子を１１２５℃以上に加熱焼成して、嵩比重１.０以上、比表面積０.１ｍ2/ｇ以下にする製造方法、および上記方法によって製造され、光透過性が焼成前の乾燥粒子より低いことを特徴とする合成シリカガラス粉末。
【選択図】図４Provided is a method capable of economically producing a synthetic silica glass powder with less spherical impurities, and a spherical synthetic silica glass powder produced by this method.
A method for producing a synthetic silica glass powder, characterized in that a synthesized siliceous gel is spray-dried to be spheronized, and the spherical dry particles are baked to vitrify, preferably spherical dry particles. By heating to 1125 ° C. or higher to produce a bulk specific gravity of 1.0 or more and a specific surface area of 0.1 m 2 / g or less, and the light transmittance is lower than that of dried particles before firing. Synthetic silica glass powder characterized by
[Selection] Figure 4
Description
本発明は、球状の不純物が少ない合成シリカガラス粉末を経済的に製造することができる方法と、この方法によって製造した球状の合成シリカガラス粉末に関する。 The present invention relates to a method capable of economically producing a synthetic silica glass powder with less spherical impurities and a spherical synthetic silica glass powder produced by this method.
半導体用途のシリコン単結晶の製造に用いる石英ガラスルツボは、以前は天然石英粉末を原料として製造されていたが、天然石英は精製しても金属不純物を完全には取除くことができないので、高純度化のため、合成石英粉末が用いられるようになり、近年は、ルツボ外側部分を天然石、ルツボ内周部分を合成石英を原料として製造したルツボが用いられている。合成石英は金属不純物が極めて少ないので、高純度のシリコン単結晶を引上げることができる。 Silica glass crucibles used for the production of silicon single crystals for semiconductors were previously manufactured using natural quartz powder as raw material. However, natural quartz cannot be completely removed even if refined quartz is refined. Synthetic quartz powder has come to be used for purification. In recent years, a crucible manufactured using natural stone for the outer part of the crucible and synthetic quartz for the inner peripheral part of the crucible has been used. Since synthetic quartz has very few metal impurities, it can pull up high-purity silicon single crystals.
この高純度の合成非晶質シリカ粉末を製造する方法としては、高純度の四塩化珪素を水で加水分解させ、生成したシリカゲルを乾燥、整粒、焼成して合成非晶質シリカ粉末を得る方法が知られている（特許文献１など）。また、珪酸エステル等のアルコキシシランを酸とアルカリの存在下で加水分解してゲル化させ、得られたゲルを乾燥、粉砕後、焼成することにより合成非晶質シリカ粉末を得る方法が知られている（特許文献２，３など）。 As a method for producing this high-purity synthetic amorphous silica powder, high-purity silicon tetrachloride is hydrolyzed with water, and the resulting silica gel is dried, sized and fired to obtain a synthetic amorphous silica powder. A method is known (for example, Patent Document 1). Also known is a method of obtaining a synthetic amorphous silica powder by hydrolyzing an alkoxysilane such as a silicate ester in the presence of an acid and an alkali to form a gel, and drying, grinding and firing the resulting gel. (Patent Documents 2, 3, etc.).
上記文献に記載されている従来の合成シリカガラスの製造方法によれば、石英ガラスルツボなどに使用されるガラス粉末を得るには、ゲル化した合成シリカを乾燥後に粉砕する工程が必要であり、粉砕に手間がかかり、しかも形状が不規則であり、球状粒子を得ることができない。さらに、粉砕装置から不純物が混入する懸念があり、粉砕のコストもかかる。 According to the conventional method for producing a synthetic silica glass described in the above-mentioned document, in order to obtain a glass powder used for a quartz glass crucible or the like, a step of pulverizing the gelated synthetic silica after drying is required. Grinding takes time, and the shape is irregular, and spherical particles cannot be obtained. Furthermore, there is a concern that impurities are mixed from the pulverizer, and the cost of pulverization is also high.
本発明は従来の製造方法における上記問題を解決したものであり、シリカ原料をゲル化した後に、粉砕工程を必要とせずに、球状のシリカガラス粉末粒子を経済的に製造する方法を提供する。 This invention solves the said problem in the conventional manufacturing method, and provides the method of manufacturing spherical silica glass powder particle | grains economically without requiring a grinding | pulverization process after gelatinizing a silica raw material.
本発明は、以下の構成によって上記課題を解決した合成シリカガラス粉末とその製造方法に関する。
〔１〕合成したシリカ質のゲルをスプレー熱風乾燥して球状化し、この球状乾燥粒子を焼成してガラス化することを特徴とする合成シリカガラス粉末の製造方法。
〔２〕この球状乾燥粒子を１１２５℃以上に加熱焼成して、嵩比重１.０以上、比表面積０.１ｍ2/ｇ以下にする請求項１に記載する合成シリカガラス粉末の製造方法。
〔３〕請求項１または請求項２の方法によって製造され、光透過性が焼成前の乾燥粒子より低いことを特徴とする合成シリカガラス粉末。
The present invention relates to a synthetic silica glass powder and a method for producing the same, which have solved the above problems with the following constitution.
[1] A method for producing a synthetic silica glass powder, characterized in that the synthesized siliceous gel is spray-dried with hot air to spheroidize, and the spherical dried particles are baked and vitrified.
[2] The method for producing a synthetic silica glass powder according to claim 1, wherein the spherical dry particles are heated and fired to 1125 ° C. or more to obtain a bulk specific gravity of 1.0 or more and a specific surface area of 0.1 m 2 / g or less.
[3] A synthetic silica glass powder produced by the method of claim 1 or 2 and having a light transmittance lower than that of dried particles before firing.
本発明の製造方法によれば、シリカ原料をゲル化した後に、粉砕工程を必要とせずに、球状の合成シリカガラス粉末粒子を得ることができる。本発明の製造方法は経済的であり、低コストで不純物の少ない高純度のシリカガラス粉末を製造することができる。 According to the production method of the present invention, spherical synthetic silica glass powder particles can be obtained without requiring a pulverization step after gelling the silica raw material. The production method of the present invention is economical and can produce a high-purity silica glass powder with low impurities and low impurities.
本発明の方法によって製造したシリカガラス粉末は、スプレー熱風乾燥することによって球状粒子を得ることができ、この粒子は粉砕した粉に比べて格段に球形のものが得られるので、例えば、石英ガラスルツボの原料として好適である。
また、本発明の製造方法に係るシリカガラス粉末はガラス質でありながら、光透過性が焼成前の乾燥粒子より低い特徴を有する。
The silica glass powder produced by the method of the present invention can obtain spherical particles by spray hot air drying, and the particles are much more spherical than the pulverized powder. It is suitable as a raw material.
In addition, the silica glass powder according to the production method of the present invention has a characteristic that its light transmittance is lower than that of dried particles before firing, although it is vitreous.
以下、本発明を実施形態に基づいて具体的に説明する。
本発明の製造方法は、合成したシリカ質のゲルをスプレー熱風乾燥して球状化し、この球状乾燥粒子を焼成してガラス化することを特徴とする合成シリカガラス粉末の製造方法である。
Hereinafter, the present invention will be specifically described based on embodiments.
The production method of the present invention is a method for producing a synthetic silica glass powder, characterized in that a synthesized siliceous gel is spray-dried with hot air to spheroidize, and the spherical dry particles are baked and vitrified.
〔シリカ質ゲルの合成工程〕
原料となるシリカ質ゲルは、（イ）四塩化珪素の加水分解、（ロ）テトラメトキシシランの加水分解、（ハ）ヒュームドシリカのゲル化などによって合成することができる。
[Synthetic process of siliceous gel]
The siliceous gel as a raw material can be synthesized by (i) hydrolysis of silicon tetrachloride, (b) hydrolysis of tetramethoxysilane, (c) gelation of fumed silica, or the like.
（イ）四塩化珪素の加水分解
四塩化珪素１molに対して、４５〜８０molに相当する量の超純水を容器内に入れ、窒素、アルゴン等の雰囲気にて、温度を２０〜４５℃に保持して攪拌しながら、四塩化珪素を容器内の超純水に添加して加水分解させる。四塩化珪素を添加してから０.５〜６時間攪拌を継続し、シリカ質のゲルを生成させる。このとき、攪拌速度は１００〜３００ｒｐｍの範囲にするのが好ましい。
(I) Hydrolysis of silicon tetrachloride An amount of ultrapure water equivalent to 45 to 80 mol is put into a container with respect to 1 mol of silicon tetrachloride, and the temperature is set to 20 to 45 ° C. in an atmosphere of nitrogen, argon or the like. While being held and stirred, silicon tetrachloride is added to ultrapure water in the container to cause hydrolysis. Stirring is continued for 0.5 to 6 hours after the addition of silicon tetrachloride to produce a siliceous gel. At this time, the stirring speed is preferably in the range of 100 to 300 rpm.
（ロ）テトラメトキシシランの加水分解
テトラメトキシシラン１molに対して、超純水０.５〜３mol、エタノール０.５〜３molを容器内に入れ、窒素、アルゴン等の雰囲気にて、温度を６０℃に保持して攪拌しながら、テトラメキシシランを容器内の超純水とエタノールの混合液に添加して加水分解させる。テトラメトキシシランを添加してから５〜１２０分間、撹拌した後に、テトラメトキシラン１molに対して１〜５０molの超純水を更に添加し、１〜１２時間攪拌を継続し、シリカ質のゲルを生成させる。このとき、攪拌速度は１００〜３００rpmの範囲にするのが好ましい。
(B) Hydrolysis of tetramethoxysilane With respect to 1 mol of tetramethoxysilane, 0.5-3 mol of ultrapure water and 0.5-3 mol of ethanol are put in a container, and the temperature is set to 60 in an atmosphere of nitrogen, argon or the like. While maintaining the temperature at a temperature of stirring, tetramethylsilane is added to a mixed liquid of ultrapure water and ethanol in the container to cause hydrolysis. After stirring for 5 to 120 minutes after adding tetramethoxysilane, 1 to 50 mol of ultrapure water is further added to 1 mol of tetramethoxylane, and stirring is continued for 1 to 12 hours. Generate. At this time, the stirring speed is preferably in the range of 100 to 300 rpm.
（ハ）ヒュームドシリカのゲル化
ヒュームドシリカ（平均粒径Ｄ50：0.007〜0.030μｍ、比表面積：50〜380m2/g）１molに対して、超純水９.５〜２０.０molを容器内に入れ、窒素、アルゴン等の雰囲気にて、温度を１０℃〜３０℃に保持して攪拌しながら、ヒュームドシリカを容器内の超純水に添加する。ヒュームドシリカを添加してから０.５〜６時間攪拌を継続し、シリカ質のゲルを生成させる。このとき、攪拌速度は１０〜５０rpmの範囲にするのが好ましい。
(C) Gelled fumed silica of fumed silica (average particle diameter D50: 0.007 to 0.030 μm, specific surface area: 50 to 380 m 2 / g) 1 mol of ultrapure water is contained in a container. The fumed silica is added to the ultrapure water in the container while stirring and maintaining the temperature at 10 ° C. to 30 ° C. in an atmosphere of nitrogen, argon or the like. Stirring is continued for 0.5 to 6 hours after the fumed silica is added to produce a siliceous gel. At this time, the stirring speed is preferably in the range of 10 to 50 rpm.
〔スプレー熱風乾燥工程〕
上記合成シリカ質ゲルを水分調整してスラリーにし、このシリカ質ゲルのスラリーをに熱風中にスプレー噴霧して乾燥し、球状のシリカ粒子にする。
[Spray hot air drying process]
The synthetic siliceous gel is adjusted to moisture to form a slurry, and the slurry of siliceous gel is sprayed into hot air and dried to form spherical silica particles.
スラリーのシリカ濃度はスプレー噴霧に適する濃度であればよく、例えば１５wt％〜３０wt％程度である。スラリーを噴霧する熱風の温度は、噴霧された液滴が適度に乾燥される温度であればよく、例えば、１８０℃〜２００℃である。 The silica concentration of the slurry may be a concentration suitable for spraying and is, for example, about 15 wt% to 30 wt%. The temperature of the hot air for spraying the slurry may be a temperature at which the sprayed droplets are appropriately dried, and is, for example, 180 ° C. to 200 ° C.
スプレー噴霧の手段としては一般のスプレードライヤーを用いることができる。スプレー方法としては、ノズルから噴霧する方法、あるいは回転ディスクにスラリーを注入して噴霧させるなど種々のタイプのスプレー方法を利用することができ、何れも目的の粒径などになるように噴霧条件に調整すればよい。ノズルから噴霧する方法は加圧ノズルでもよく、二流体ノズルでもよい。 As a spraying means, a general spray dryer can be used. As the spraying method, various types of spraying methods such as spraying from a nozzle or injecting slurry into a rotating disk and spraying can be used. Adjust it. The method of spraying from the nozzle may be a pressurized nozzle or a two-fluid nozzle.
〔加熱焼成工程〕
スプレー乾燥によって得た球状粒子を、１１２５℃以上に加熱焼成して、嵩比重１.０以上、比表面積０.１ｍ2/ｇ以下にガラス化する。焼成前の状態を図１に示す。焼成温度１０００℃、焼成温度１１２５℃、焼成温度１２００℃の焼成状態を図２〜図４に示す。また、焼成温度と嵩密度の関係を図５に示す。焼成温度と比表面積の関係を図６に示す。焼成温度と光透過範囲の関係を図７に示す。１２５０℃で焼成したシリカガラス粉末の粒度分布を図８に示す。
[Heating and firing process]
Spherical particles obtained by spray drying are heated and fired to 1125 ° C. or higher to vitrify to a bulk specific gravity of 1.0 or more and a specific surface area of 0.1 m 2 / g or less. The state before firing is shown in FIG. FIGS. 2 to 4 show firing states at a firing temperature of 1000 ° C., a firing temperature of 1125 ° C., and a firing temperature of 1200 ° C. Moreover, the relationship between a calcination temperature and a bulk density is shown in FIG. FIG. 6 shows the relationship between the firing temperature and the specific surface area. FIG. 7 shows the relationship between the firing temperature and the light transmission range. The particle size distribution of the silica glass powder fired at 1250 ° C. is shown in FIG.
焼成方法は、通常は石英製の容器に充填してバッチで焼成すればよい。また、回転式のキルンで連続的に焼いてもよく、この焼成物はさらさらの分散状態になる。焼成の雰囲気は、ガラス内部の気泡の除去効果を高めるには、焼成後半に減圧してもよく、さらには不活性ガスで置換して焼成してもよい。 As a firing method, a quartz container is usually filled and fired in a batch. Moreover, you may bake continuously with a rotary kiln and this baked product will be in the state of smooth dispersion. In order to enhance the effect of removing bubbles in the glass, the firing atmosphere may be reduced in pressure in the latter half of the firing, or further replaced with an inert gas and fired.
図１に示すように焼成前の乾燥粒子はガラス化していない。図２に示すように１０００℃で焼成してもガラス化は不十分である。一方、図３に示すように１１２５℃で焼成したものは次第にガラス化し、図４に示すように１２００℃で焼成したものはガラス化が進行している。 As shown in FIG. 1, the dried particles before firing are not vitrified. As shown in FIG. 2, vitrification is insufficient even when fired at 1000 ° C. On the other hand, as shown in FIG. 3, the one fired at 1125 ° C. is gradually vitrified, and the one fired at 1200 ° C. as shown in FIG. 4 is vitrified.
焼成温度とガラス化の程度は図５および図６にも示されており、図５に示すように、焼成温度が１１００℃を超えると急激に嵩比重が増加し、１１２５℃以上で焼成すると嵩比重が１.０以上になる。また、図６に示すように、焼成温度が１１００℃を超えると急激に比表面積が小さくなり、１１２５℃以上で焼成すると比表面積は０.１ｍ2/ｇ以下になる。 The firing temperature and the degree of vitrification are also shown in FIGS. 5 and 6. As shown in FIG. 5, when the firing temperature exceeds 1100 ° C., the bulk specific gravity suddenly increases. Specific gravity becomes 1.0 or more. Further, as shown in FIG. 6, the specific surface area rapidly decreases when the firing temperature exceeds 1100 ° C., and the specific surface area becomes 0.1 m 2 / g or less when fired at 1125 ° C. or higher.
また、本発明の方法によって製造した合成シリカガラス粉末は、シャープな粒度分布を有しており、図８に示すように、１２５０℃で焼成したシリカガラス粉末の粒径は約６０μmから約１２０μmに集中しており、平均粒径Ｄ50は約１１０μmである。 In addition, the synthetic silica glass powder produced by the method of the present invention has a sharp particle size distribution. As shown in FIG. 8, the particle size of the silica glass powder fired at 1250 ° C. is about 60 μm to about 120 μm. The average particle size D50 is about 110 μm.
さらに、本発明の方法によって製造した合成シリカガラス粉末は、ガラス質でありながら、光透過性が焼成前の乾燥粒子より低い性質を有する。本発明の合成シリカガラス粉末をガラス瓶に入れ、ガラス瓶の底から光（赤色レーザ光）を照射して、ガラス粉末が赤色に輝く範囲（ガラス底からの高さ）を目視観察すると、図７に示すように、焼成温度が９００℃以下の場合（ガラス化前）には、約１９mmの範囲まで光が透過するが、焼成温度が１０００℃を超えると光の透過範囲が急激に低下し、焼成温度が１２５０℃以上のガラス化が進行した状態では光の透過範囲は約１３mmから約１２mmに低下し、焼成前の約６０％程度に低下する。 Furthermore, the synthetic silica glass powder produced by the method of the present invention has a property that light permeability is lower than that of dried particles before firing, while being vitreous. When the synthetic silica glass powder of the present invention is put into a glass bottle, light (red laser light) is irradiated from the bottom of the glass bottle, and the range in which the glass powder shines red (height from the glass bottom) is visually observed, FIG. As shown, when the firing temperature is 900 ° C. or lower (before vitrification), the light is transmitted to a range of about 19 mm, but when the firing temperature exceeds 1000 ° C., the light transmission range is drastically lowered and the firing is performed. In a state where vitrification at a temperature of 1250 ° C. or higher has progressed, the light transmission range is reduced from about 13 mm to about 12 mm, and is reduced to about 60% before firing.
以下、本発明の実施例を示す。
〔実施例１〕
ヒュームドシリカ（商品名アエロジルAE50）をゲル化し、濃度１５wt％に水分調整してシリカスラリーにした。このスラリーをスプレードライヤーを用い、入口温度２００℃、出口温度９２度の熱風中に、加圧ノズル（ノズル径１mm）から噴霧圧１.３ＭPaの圧力で乾燥室の下方から上方に向けて噴霧し、平均粒径１７０μmの燥球状粒子を得た。この乾燥粒子を空気中で１３時間焼成した。
焼成前の乾燥粒子を図１に示す。焼成温度１０００℃の状態を図２に示す。焼成温度１１２５℃の状態を図３に示す。焼成温度１２００℃の状態を図４に示す。焼成温度と嵩密度の関係を図５に示す。焼成温度と比表面積の関係を図６に示す。焼成温度と光透過範囲の関係を図７に示す。１２５０℃で焼成したシリカガラス粉末の粒度分布を図８に示す。
Examples of the present invention will be described below.
[Example 1]
Fumed silica (trade name Aerosil AE50) was gelled and adjusted to a water content of 15 wt% to form a silica slurry. This slurry is sprayed from the bottom of the drying chamber to the top at a pressure of 1.3 MPa from a pressure nozzle (nozzle diameter 1 mm) in hot air with an inlet temperature of 200 ° C. and an outlet temperature of 92 ° C. Dry spherical particles having an average particle size of 170 μm were obtained. The dried particles were fired in air for 13 hours.
The dried particles before firing are shown in FIG. A state at a firing temperature of 1000 ° C. is shown in FIG. A state at a firing temperature of 1125 ° C. is shown in FIG. A state at a firing temperature of 1200 ° C. is shown in FIG. The relationship between the firing temperature and the bulk density is shown in FIG. FIG. 6 shows the relationship between the firing temperature and the specific surface area. FIG. 7 shows the relationship between the firing temperature and the light transmission range. The particle size distribution of the silica glass powder fired at 1250 ° C. is shown in FIG.
図２に示すように１０００℃で焼成してもガラス化は不十分である。図３に示すように１１２５℃で焼成したものは次第にガラス化しており、図４に示すように１２００℃で焼成したものはガラス化が進行している。これに対応し、図５に示すように、焼成温度が１１００℃を超えると急激に嵩比重が増加し、１１２５℃以上で焼成すると嵩比重が１.０以上になる。また、図６に示すように、焼成温度が１１００℃を超えると急激に比表面積が小さくなり、１１２５℃以上で焼成すると比表面積は０.１ｍ2/ｇ以下になる。このように、焼成温度が１１２５℃で物性が大きく変化しており、この温度がガラス化の始まる変局点であることを示している。 As shown in FIG. 2, vitrification is insufficient even when fired at 1000 ° C. As shown in FIG. 3, the one fired at 1125 ° C. is gradually vitrified, and as shown in FIG. 4, the one fired at 1200 ° C. is vitrified. Correspondingly, as shown in FIG. 5, when the firing temperature exceeds 1100 ° C., the bulk specific gravity suddenly increases, and when fired at 1125 ° C. or higher, the bulk specific gravity becomes 1.0 or higher. Further, as shown in FIG. 6, the specific surface area rapidly decreases when the firing temperature exceeds 1100 ° C., and the specific surface area becomes 0.1 m 2 / g or less when fired at 1125 ° C. or higher. Thus, the physical properties change greatly at a firing temperature of 1125 ° C., indicating that this temperature is the inflection point at which vitrification begins.
図８に示すように、１２５０℃で焼成したシリカガラス粉末の粒径は約６０μmから約１２０μmに集中しており、平均粒径Ｄ50は約１１０μmである。また、図２(Ａ)〜(Ｃ)に示すように、焼成温度１１２５℃で製造したガラス粒子は、空洞が外に開いたクラインの壷型の球状粒子であるが、１２００℃以上で焼成すると空洞が閉じた球状粒子になる。 As shown in FIG. 8, the particle diameter of the silica glass powder fired at 1250 ° C. is concentrated from about 60 μm to about 120 μm, and the average particle diameter D50 is about 110 μm. As shown in FIGS. 2A to 2C, glass particles produced at a firing temperature of 1125 ° C. are Klein-shaped spherical particles having cavities open to the outside, but when fired at 1200 ° C. or higher. Spherical particles with closed cavities.
製造した合成シリカガラス粉末をガラス瓶に入れ、ガラス瓶の底から光（赤色レーザ光）を照射して、ガラス粉末が赤色に輝く範囲（ガラス底からの高さ）を目視観察すると、図７に示すように、焼成温度が９００℃以下の場合（ガラス化前）には、約１９mmの範囲まで光が透過するが、焼成温度が１０００℃を超えると光の透過範囲が急激に低下し、焼成温度が１２５０℃以上のガラス化が進行した状態では光の透過範囲は約１３mmから約１２mmに低下し、焼成前の約６０％程度に低下する。 The manufactured synthetic silica glass powder is put into a glass bottle, irradiated with light (red laser light) from the bottom of the glass bottle, and the range where the glass powder shines red (height from the glass bottom) is visually observed, as shown in FIG. Thus, when the firing temperature is 900 ° C. or lower (before vitrification), light is transmitted to a range of about 19 mm. However, when the firing temperature exceeds 1000 ° C., the light transmission range is rapidly reduced, and the firing temperature is reduced. However, in a state where vitrification at 1250 ° C. or higher has progressed, the light transmission range is reduced from about 13 mm to about 12 mm, and is reduced to about 60% before firing.
〔実施例２〕
ヒュームドシリカ（商品名アエロジルAE50）をゲル化し、濃度３０wt％に水分調整してシリカスラリーにした。このスラリーをディスク型のスプレードライヤーを用い、入口温度１８０℃、出口温度１００℃の熱風中に、ピン型ディスクで上方からアトマイズ（噴霧）し、平均粒径１７０μmの燥球状粒子を得た。この乾燥粒子を空気中で１３時間焼成した。
この乾燥粒子を用いて実施例１と同様に加熱焼成を行い、合成シリカガラス粉末を得た。このシリカガラス粉末は、図２〜図８に示すものとほぼ同等の物性を有するものであった。
[Example 2]
Fumed silica (trade name Aerosil AE50) was gelled and adjusted to a water concentration of 30 wt% to form a silica slurry. This slurry was atomized (sprayed) from above with a pin type disk in hot air having an inlet temperature of 180 ° C. and an outlet temperature of 100 ° C. using a disk type spray dryer to obtain dry spherical particles having an average particle size of 170 μm. The dried particles were fired in air for 13 hours.
The dried particles were used for heating and firing in the same manner as in Example 1 to obtain a synthetic silica glass powder. This silica glass powder had substantially the same physical properties as those shown in FIGS.
Claims (3)
A method for producing a synthetic silica glass powder, characterized in that the synthesized siliceous gel is spray-dried with hot air to spheroidize, and the spherical dry particles are baked to vitrify.
The method for producing a synthetic silica glass powder according to claim 1, wherein the spherical dry particles are heated and fired to 1125 ° C or higher to obtain a bulk specific gravity of 1.0 or more and a specific surface area of 0.1 m 2 / g or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010078940A JP2011207719A (en) | 2010-03-30 | 2010-03-30 | Synthetic amorphous silica powder and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010078940A JP2011207719A (en) | 2010-03-30 | 2010-03-30 | Synthetic amorphous silica powder and method for producing the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2011207719A true JP2011207719A (en) | 2011-10-20 |
Family
ID=44939201
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2010078940A Withdrawn JP2011207719A (en) | 2010-03-30 | 2010-03-30 | Synthetic amorphous silica powder and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2011207719A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016069275A (en) * | 2014-09-29 | 2016-05-09 | ヘレーウス クヴァルツグラース ゲゼルシャフト ミット ベシュレンクテル ハフツング ウント コンパニー コマンディートゲゼルシャフトＨｅｒａｅｕｓ Ｑｕａｒｚｇｌａｓ ＧｍｂＨ ＆ Ｃｏ． ＫＧ | Method for producing synthetic quartz glass of SiO2 granule and SiO2 granule suitable for the production method |
| WO2017103125A1 (en) * | 2015-12-18 | 2017-06-22 | Heraeus Quarzglas Gmbh & Co. Kg | Spray granulation of silica during the production of silica glass |
| JP2017210403A (en) * | 2016-05-24 | 2017-11-30 | ヘレーウス クヴァルツグラース ゲゼルシャフト ミット ベシュレンクテル ハフツング ウント コンパニー コマンディートゲゼルシャフトＨｅｒａｅｕｓ Ｑｕａｒｚｇｌａｓ ＧｍｂＨ ＆ Ｃｏ． ＫＧ | Production method of opaque quartz glass containing pore |
| CN110803860A (en) * | 2019-11-19 | 2020-02-18 | 新沂北美高科耐火材料有限公司 | Preparation method of electronic-grade spherical fused quartz refractory material |
| US10618833B2 (en) | 2015-12-18 | 2020-04-14 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a synthetic quartz glass grain |
| JP2020079165A (en) * | 2018-11-12 | 2020-05-28 | 花王株式会社 | Hollow silica particles and method for producing the same |
| US10676388B2 (en) | 2015-12-18 | 2020-06-09 | Heraeus Quarzglas Gmbh & Co. Kg | Glass fibers and pre-forms made of homogeneous quartz glass |
| US10730780B2 (en) | 2015-12-18 | 2020-08-04 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a multi-chamber oven |
| US11236002B2 (en) | 2015-12-18 | 2022-02-01 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of an opaque quartz glass body |
| US11299417B2 (en) | 2015-12-18 | 2022-04-12 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a melting crucible of refractory metal |
| US11339076B2 (en) | 2015-12-18 | 2022-05-24 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of carbon-doped silicon dioxide granulate as an intermediate in the preparation of quartz glass |
| US11492282B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies with dew point monitoring in the melting oven |
| US11492285B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies from silicon dioxide granulate |
| US11952303B2 (en) | 2015-12-18 | 2024-04-09 | Heraeus Quarzglas Gmbh & Co. Kg | Increase in silicon content in the preparation of quartz glass |
-
2010
- 2010-03-30 JP JP2010078940A patent/JP2011207719A/en not_active Withdrawn
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3000790B1 (en) | 2014-09-29 | 2019-11-27 | Heraeus Quarzglas GmbH & Co. KG | Method for synthetic quartz-glass production from SiO2 granulate and SiO2 granulate suitable for the same |
| EP3000790B2 (en) † | 2014-09-29 | 2023-07-26 | Heraeus Quarzglas GmbH & Co. KG | Method for production of components made of synthetic quartz-glass from SiO2 granulate |
| JP2016069275A (en) * | 2014-09-29 | 2016-05-09 | ヘレーウス クヴァルツグラース ゲゼルシャフト ミット ベシュレンクテル ハフツング ウント コンパニー コマンディートゲゼルシャフトＨｅｒａｅｕｓ Ｑｕａｒｚｇｌａｓ ＧｍｂＨ ＆ Ｃｏ． ＫＧ | Method for producing synthetic quartz glass of SiO2 granule and SiO2 granule suitable for the production method |
| US10029938B2 (en) | 2014-09-29 | 2018-07-24 | Heraeus Quarzglas Gmbh & Co. Kg | Method for producing synthetic quartz glass of SiO2 granulate and SiO2 granulate suited therefor |
| US11492282B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies with dew point monitoring in the melting oven |
| US11236002B2 (en) | 2015-12-18 | 2022-02-01 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of an opaque quartz glass body |
| US10618833B2 (en) | 2015-12-18 | 2020-04-14 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a synthetic quartz glass grain |
| US11952303B2 (en) | 2015-12-18 | 2024-04-09 | Heraeus Quarzglas Gmbh & Co. Kg | Increase in silicon content in the preparation of quartz glass |
| US10676388B2 (en) | 2015-12-18 | 2020-06-09 | Heraeus Quarzglas Gmbh & Co. Kg | Glass fibers and pre-forms made of homogeneous quartz glass |
| US10730780B2 (en) | 2015-12-18 | 2020-08-04 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a multi-chamber oven |
| US11053152B2 (en) | 2015-12-18 | 2021-07-06 | Heraeus Quarzglas Gmbh & Co. Kg | Spray granulation of silicon dioxide in the preparation of quartz glass |
| WO2017103125A1 (en) * | 2015-12-18 | 2017-06-22 | Heraeus Quarzglas Gmbh & Co. Kg | Spray granulation of silica during the production of silica glass |
| US11299417B2 (en) | 2015-12-18 | 2022-04-12 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a melting crucible of refractory metal |
| US11339076B2 (en) | 2015-12-18 | 2022-05-24 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of carbon-doped silicon dioxide granulate as an intermediate in the preparation of quartz glass |
| US11708290B2 (en) | 2015-12-18 | 2023-07-25 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a multi-chamber oven |
| US11492285B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies from silicon dioxide granulate |
| JP2017210403A (en) * | 2016-05-24 | 2017-11-30 | ヘレーウス クヴァルツグラース ゲゼルシャフト ミット ベシュレンクテル ハフツング ウント コンパニー コマンディートゲゼルシャフトＨｅｒａｅｕｓ Ｑｕａｒｚｇｌａｓ ＧｍｂＨ ＆ Ｃｏ． ＫＧ | Production method of opaque quartz glass containing pore |
| JP7132827B2 (en) | 2018-11-12 | 2022-09-07 | 花王株式会社 | Hollow silica particles and method for producing the same |
| JP2020079165A (en) * | 2018-11-12 | 2020-05-28 | 花王株式会社 | Hollow silica particles and method for producing the same |
| CN110803860A (en) * | 2019-11-19 | 2020-02-18 | 新沂北美高科耐火材料有限公司 | Preparation method of electronic-grade spherical fused quartz refractory material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2011207719A (en) | Synthetic amorphous silica powder and method for producing the same | |
| CN102652109B (en) | Synthesis amorphous silicon di-oxide powder and manufacture method thereof | |
| JP6698585B2 (en) | Method for producing opaque quartz glass containing pores | |
| MX2009002123A (en) | Sol-gel process. | |
| JPH02275713A (en) | Production of spherical silica grain | |
| JP2009137836A (en) | Method for producing glassy monolith via sol-gel process | |
| JPH072513A (en) | Method for producing synthetic quartz glass powder | |
| JP2011157262A (en) | Synthetic amorphous silica powder and method for producing same | |
| TWI780379B (en) | Manufacturing method of opaque quartz glass | |
| MX2007010811A (en) | Process for the production of monoliths by means of the invert sol-gel process. | |
| JPS62176928A (en) | Production of quartz glass powder | |
| WO2010015658A1 (en) | Sol-gel process for producing monolithic articles of vitreous silica | |
| JP5941774B2 (en) | Synthetic silica glass powder and method for producing the same | |
| JP7480659B2 (en) | Transparent glass manufacturing method | |
| JPS6296313A (en) | Production of high-purity spherical silica filler | |
| JP2022052497A (en) | Granulated silica powder and production method of granulated silica powder | |
| JP3318946B2 (en) | Powdery dry gel, silica glass powder, and method for producing silica glass melt molded article | |
| JP2675819B2 (en) | Manufacturing method of quartz glass | |
| KR100722378B1 (en) | Method for producing transparent silica glass | |
| JP4389890B2 (en) | Silica gel and its production method, synthetic quartz glass powder and its production method, and synthetic quartz glass molded body and its production method | |
| JP2023135320A (en) | Method for producing granulated silica powder | |
| JP4322262B2 (en) | Method for producing synthetic quartz glass powder | |
| JP3847819B2 (en) | Method for producing synthetic quartz glass powder | |
| JPH0283224A (en) | Production of synthetic quartz glass powder | |
| JPH10101322A (en) | Silica gel, synthetic quartz glass powder, method for producing the same, and method for producing quartz glass compact |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 20130604 |