JP2019172562A - Manufacturing method of quartz glass - Google Patents
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Abstract
Description
本明細書によって開示される技術は、石英ガラスの製造方法に関する。 The technique disclosed by this specification is related with the manufacturing method of quartz glass.
シリカ粉とバインダーとを混練し、成形して得られた成形体に脱脂処理、純化処理を施した後、ガラス化して石英ガラスを製造する方法が知られている（特許文献１参照）。 A method is known in which silica powder and a binder are kneaded and formed into a molded product obtained by degreasing and purification, and then vitrified to produce quartz glass (see Patent Document 1).
上記のような製造方法は、成形体に脱脂処理を施してバインダー成分を除去する工程が必要になるなど、工程数が多く複雑になりがちであった。 The manufacturing method as described above tends to be complicated due to a large number of steps, such as a step of degreasing the molded body to remove the binder component.
本明細書によって開示される石英ガラスの製造方法は、シリカ粉末と水のみを混合して混合物を得る混合工程と、前記混合物を成形して成形体を得る成形工程と、前記成形体を加熱処理して石英ガラスを得る加熱処理工程とを含む。このような方法によれば、成形体に脱脂処理を施してバインダー成分を除去する工程が不要となり、製造工程を簡素化することができる。 The method for producing quartz glass disclosed in the present specification includes a mixing step of mixing only silica powder and water to obtain a mixture, a forming step of forming the mixture to obtain a formed body, and heat-treating the formed body. And a heat treatment step for obtaining quartz glass. According to such a method, the process which removes a binder component by performing a degreasing process to a molded object becomes unnecessary, and a manufacturing process can be simplified.
本明細書によって開示される石英ガラスの製造方法によれば、簡易な工程で石英ガラスを得ることができる。 According to the method for producing quartz glass disclosed in the present specification, quartz glass can be obtained by a simple process.
実施形態の石英ガラスの製造方法は、シリカ粉末と水のみを混合して混合物を得る混合工程と、前記混合物を成形して成形体を得る成形工程と、前記成形体を加熱処理して石英ガラスを得る加熱処理工程とを含む。 The method for producing quartz glass according to the embodiment includes a mixing step of mixing only silica powder and water to obtain a mixture, a forming step of forming the mixture to obtain a formed body, and a heat treatment of the formed body to produce quartz glass. And a heat treatment step to obtain
混合工程においては、シリカ粉末と水のみを混合し、バインダーを混合しない。バインダーを用いないことによって、成形体からバインダー成分を除去する脱脂工程を省略することができ、製造工程が簡素化される。用いられるシリカ粉末の平均一次粒子径は、７ｎｍ以上１００ｎｍ以下であることが好ましく、７ｎｍ以上５０ｎｍ以下であることがより好ましく、２２ｎｍ以上５０ｎｍ以下であることがさらに好ましく、５０ｎｍであることが最も好ましい。さらに、シリカ粉末の平均一次粒子径が５０ｎｍである場合に、水を、シリカ粉末１０質量部に対して６．０９質量部以上６．２１質量部以下の割合で混合することが好ましい。 In the mixing step, only silica powder and water are mixed, and the binder is not mixed. By not using a binder, the degreasing process which removes a binder component from a molded object can be skipped, and a manufacturing process is simplified. The average primary particle diameter of the silica powder used is preferably 7 nm or more and 100 nm or less, more preferably 7 nm or more and 50 nm or less, further preferably 22 nm or more and 50 nm or less, and most preferably 50 nm. . Furthermore, when the average primary particle diameter of the silica powder is 50 nm, it is preferable to mix water at a ratio of 6.09 parts by mass to 6.21 parts by mass with respect to 10 parts by mass of the silica powder.
また、混合工程は、シリカ粉末と水とを減圧下で混合する工程を含むことが好ましく、シリカ粉末と水とを真空状態で混合する工程を含むことがさらに好ましい。減圧下または真空状態での混合は、例えば、シリカ粉末と水とを、真空撹拌機を用いて攪拌することにより行うことができる。これにより、脱泡しつつ混合を行うことができるので、気泡が入らない良好な成形体を得ることができる。この場合には、混合工程完了後の混合物が、水を、シリカ粉末１０質量部に対して５．３２質量部以上５．６７質量部以下の割合で含有することが好ましい。 The mixing step preferably includes a step of mixing silica powder and water under reduced pressure, and more preferably includes a step of mixing silica powder and water in a vacuum state. Mixing under reduced pressure or in a vacuum state can be performed, for example, by stirring silica powder and water using a vacuum stirrer. Thereby, since it can mix while defoaming, the favorable molded object which a bubble does not enter can be obtained. In this case, it is preferable that the mixture after the completion of the mixing step contains water at a ratio of 5.32 parts by mass to 5.67 parts by mass with respect to 10 parts by mass of the silica powder.
成形工程においては、例えばシリコーン型または金型を使用した注型成形を行うことができる。あるいは、金型を用いてプレス成形を行っても良い。
また、石英ガラスが光学部材である場合には、光学部材の形状に対応する形状を有する型を用いて成形を行うことが好ましい。これにより、所望の光学部材の形状を有する成形体を得て、これを加熱処理するだけで光学部材を得ることができるので、石英ガラスの塊から削りや研磨でレンズ部材の形状を作りだす場合と比較して、製造工程が簡素となる。
In the molding process, cast molding using, for example, a silicone mold or a mold can be performed. Alternatively, press molding may be performed using a mold.
Further, when quartz glass is an optical member, it is preferable to perform molding using a mold having a shape corresponding to the shape of the optical member. This makes it possible to obtain a molded body having the shape of a desired optical member, and to obtain an optical member simply by heat-treating it, so that the shape of the lens member is created by shaving or polishing from a lump of quartz glass In comparison, the manufacturing process is simplified.
加熱処理工程は、ガラス化のために、例えば成形体を不活性ガス雰囲気中、または真空状態、更には大気中で、９００℃〜１４００℃の温度領域で加熱することにより行うことができる。特に、加熱処理を不活性ガス雰囲気下で行うことが好ましい。石英ガラスの表面が、大気中の不純物との反応によって変質することを回避できるためである。 For vitrification, the heat treatment step can be performed, for example, by heating the molded body in an inert gas atmosphere, in a vacuum state, or in the air in a temperature range of 900 ° C. to 1400 ° C. In particular, the heat treatment is preferably performed in an inert gas atmosphere. This is because the surface of the quartz glass can be prevented from being altered by reaction with impurities in the atmosphere.
加熱処理工程が、第１の昇温速度で所定温度まで昇温させる第１昇温工程と、第１昇温工程の後に、第１の昇温速度よりも緩やかな第２の昇温速度で昇温させる第２の昇温工程とを含むことが好ましい。第１昇温工程では、比較的早い昇温速度で昇温することで、成形体に含まれる水を加熱除去する。第２昇温工程では、比較的緩やかな昇温速度で昇温してシリカを徐々に収縮させることで、急激な加熱によるヒビや割れの発生を回避して、良好な石英ガラスを得ることができる。
より具体的には、上記の第１昇温工程における「所定温度」が９００℃以上１０００℃以下であり、第１の昇温速度が、１０℃／ｍｉｎ以上１５℃／ｍｉｎ以下であり、第２の昇温速度が３℃／ｍｉｎであることが好ましい。
なお、第１昇温工程と第２昇温工程との間に、上記所定温度で所定時間（例えば３０分〜６０分）保持する保持工程を設けてもよく、保持工程を設けなくても構わない。
The heat treatment step includes a first temperature raising step for raising the temperature to a predetermined temperature at a first temperature raising rate, and a second temperature raising rate that is slower than the first temperature raising rate after the first temperature raising step. It is preferable to include a second temperature raising step for raising the temperature. In the first temperature raising step, the water contained in the molded body is removed by heating by raising the temperature at a relatively high temperature raising rate. In the second temperature raising step, the silica is gradually shrunk by raising the temperature at a relatively slow temperature raising rate, thereby avoiding the occurrence of cracks and cracks due to abrupt heating and obtaining a good quartz glass. it can.
More specifically, the “predetermined temperature” in the first temperature raising step is 900 ° C. or higher and 1000 ° C. or lower, the first temperature rising rate is 10 ° C./min or higher and 15 ° C./min or lower, 2 is preferably 3 ° C./min.
In addition, between the 1st temperature rising process and the 2nd temperature rising process, the holding process hold | maintained for the predetermined time (for example, 30 minutes-60 minutes) at the said predetermined temperature may be provided, and it is not necessary to provide a holding process. Absent.
＜試験例＞
［使用材料］
シリカ粉末として、株式会社トクヤマ製 「シルフィル ＮＳＳ−３Ｎ（平均一次粒子径 ０．１２μｍ）」、「レオロシール ＱＳ−０９（平均一次粒子径 ２２ｎｍ）」、「レオロシール ＣＰ−１０２（平均一次粒子径 １２ｎｍ）」、「レオロシール ＱＳ−３０（平均一次粒子径 ７ｎｍ）」を使用した。
<Test example>
[Materials used]
As silica powder, “Silfil NSS-3N (average primary particle size: 0.12 μm)”, “Leoroseal QS-09 (average primary particle size: 22 nm)”, “Lerosil CP-102 (average primary particle size: 12 nm)” manufactured by Tokuyama Corporation. ”,“ Leorosil QS-30 (average primary particle size 7 nm) ”.
［試験方法］
１．試験例１〜７
各シリカ粉末を純水と混合して混合物を得た。混合する際には、真空状態での攪拌を行って混合物を得た（混合工程）。より具体的には、スターラーのない自転・公転攪拌器（攪拌機）を用い、真空状態で攪拌を行った。この攪拌により得られた混合物を、すぐに、光学レンズに対応する形状を有するシリコーン型に注入する注型成形を行って、常温状態で３日以上放置して乾燥し、φ１０ｍｍの成形体を得た（成形工程）。
なお、各試験例において、シリカ粉末の平均一次粒子径、およびシリカ粉末と純水との混合比は、表１に示すとおりである。表１において、シリカ粉末と純水との混合比は、質量比（重量比）である。
[Test method]
1. Test Examples 1-7
Each silica powder was mixed with pure water to obtain a mixture. When mixing, stirring in a vacuum state was performed to obtain a mixture (mixing step). More specifically, stirring was performed in a vacuum state using a rotation / revolution stirrer (stirrer) without a stirrer. The mixture obtained by this stirring is immediately cast-molded by injecting it into a silicone mold having a shape corresponding to the optical lens, and allowed to stand at room temperature for 3 days or more to dry, thereby obtaining a molded product having a diameter of 10 mm. (Molding process).
In each test example, the average primary particle diameter of the silica powder and the mixing ratio of the silica powder and pure water are as shown in Table 1. In Table 1, the mixing ratio of silica powder and pure water is a mass ratio (weight ratio).
得られた成形体を加熱炉内にセットし、ヘリウム雰囲気中で、以下の昇温条件で加熱を行い、ガラス化を行った（加熱処理工程；図１参照）。
まず、室温から９００℃まで、昇温速度１０℃／ｍｉｎで昇温し（第１昇温工程）、９００℃で６０分保持した。次に、９００℃から１３００℃まで、昇温速度３℃／ｍｉｎで昇温し（第２昇温工程）、１３００℃で３０分保持した。この後、室温まで冷却して、石英ガラスを得た。
The obtained molded body was set in a heating furnace, and heated in the helium atmosphere under the following temperature raising conditions to perform vitrification (heat treatment step; see FIG. 1).
First, the temperature was raised from room temperature to 900 ° C. at a rate of temperature rise of 10 ° C./min (first temperature raising step) and held at 900 ° C. for 60 minutes. Next, the temperature was raised from 900 ° C. to 1300 ° C. at a rate of temperature rise of 3 ° C./min (second temperature raising step) and held at 1300 ° C. for 30 minutes. Then, it cooled to room temperature and obtained quartz glass.
２．試験例８
加熱を真空状態で行い、第２昇温工程において１４００℃まで昇温した他は、試験例６と同様にして石英ガラスを得た。
2. Test Example 8
Quartz glass was obtained in the same manner as in Test Example 6 except that heating was performed in a vacuum state and the temperature was raised to 1400 ° C. in the second temperature raising step.
３．試験例９
加熱を大気中で行い、第２昇温工程において１３１５℃まで昇温した他は、試験例６と同様にして石英ガラスを得た。
3. Test Example 9
Quartz glass was obtained in the same manner as in Test Example 6 except that heating was performed in air and the temperature was raised to 1315 ° C. in the second temperature raising step.
［結果］
表１において、透明な石英ガラスを得られなかったものを×、透明な石英ガラスを得られたものを○、光学部材としても使用可能な品質の透明な石英ガラスを得られたものを◎として示した。なお、光学部材とは、光学レンズの他、保護ガラス（ウィンドウ）や屈折板等のレンズ以外の光学特性を有する部材を含む。
[result]
In Table 1, “X” indicates that transparent quartz glass was not obtained, “◯” indicates that transparent quartz glass was obtained, and “◎” indicates that transparent quartz glass of a quality that can be used as an optical member was obtained. Indicated. The optical member includes a member having optical characteristics other than the lens such as a protective glass (window) and a refracting plate in addition to the optical lens.
平均一次粒子径０．１２μｍ（１２０ｎｍ）のシリカ粉末を用い、シリカ粉末：純水＝１：１で混合した試験例７では、成形工程において混合物が固まらず、成形体を得ることができなかった。 In Test Example 7 in which silica powder having an average primary particle size of 0.12 μm (120 nm) was used and mixed with silica powder: pure water = 1: 1, the mixture did not solidify in the molding step, and a molded product could not be obtained. .
平均一次粒子径７ｎｍ〜２２ｎｍのシリカ粉末を用い、シリカ粉末：純水＝２：３または１：２とした試験例１〜試験例６においては、石英ガラスを得ることができた。特に、平均一次粒子径２２ｎｍのシリカ粉末を用いた場合には、いずれの混合比でも光学部材としても使用可能な品質の石英ガラスを得ることができた。また、シリカ粉末：純水＝１：２とした場合には、シリカ粉末の平均一次粒子径が７ｎｍまたは１２ｎｍであっても、光学部材としても使用可能な品質の石英ガラスを得ることができた。さらに、平均一次粒子径２２ｎｍのシリカ粉末を用い、シリカ粉末：純水＝２：３とした試験例６、８、９では、加熱条件を変えても、光学部材としても使用可能な品質の石英ガラスを得ることができた。 In Test Example 1 to Test Example 6 using silica powder having an average primary particle diameter of 7 nm to 22 nm and silica powder: pure water = 2: 3 or 1: 2, quartz glass could be obtained. In particular, when silica powder having an average primary particle diameter of 22 nm was used, it was possible to obtain quartz glass having a quality that can be used as an optical member at any mixing ratio. In addition, when silica powder: pure water = 1: 2, even if the average primary particle diameter of the silica powder is 7 nm or 12 nm, it is possible to obtain a quality quartz glass that can be used as an optical member. . Furthermore, in Test Examples 6, 8, and 9 using silica powder having an average primary particle diameter of 22 nm and silica powder: pure water = 2: 3, the quality quartz that can be used as an optical member even if the heating conditions are changed. Glass could be obtained.
＜さらに詳細に検討する試験例＞
上記の試験結果を踏まえ、シリカ粉末の好適な平均一次粒子径、および、シリカ粉末と水との好適な混合比をさらに詳細に検討する試験を行った。
<Examples to be examined in more detail>
Based on the above test results, a test was conducted in which the preferred average primary particle diameter of the silica powder and the preferred mixing ratio of the silica powder and water were examined in more detail.
［使用材料］
シリカ粉末として、以下のものを使用した。
・株式会社トクヤマ製「レオロシール」（平均一次粒子径：７ｎｍ、１２ｎｍ、２２ｎｍ）」
・株式会社トクヤマ製「シルフィル」（平均一次粒子径：１２５ｎｍ）
・堺化学工業株式会社製「Ｓｃｉｑａｓ」（平均一次粒子径：５０ｎｍ、１００ｎｍ、４００ｎｍ、７００ｎｍ、１０００ｎｍ）
[Materials used]
The following were used as the silica powder.
-"Leoro Seal" manufactured by Tokuyama Corporation (average primary particle size: 7 nm, 12 nm, 22 nm) "
-"Silfil" manufactured by Tokuyama Corporation (average primary particle size: 125 nm)
-“Sciqas” manufactured by Sakai Chemical Industry Co., Ltd. (average primary particle size: 50 nm, 100 nm, 400 nm, 700 nm, 1000 nm)
［試験方法］
４．試験例１０
シリカ粉末の平均一次粒子径、およびシリカ粉末と純水との混合比を、下記表２に示すとおりとし、試験例１と同様の手順で石英ガラスを得た。表２において、シリカ粉末と純水との混合比は、質量比（重量比）である。
[Test method]
4). Test Example 10
The average primary particle diameter of the silica powder and the mixing ratio of the silica powder and pure water were as shown in Table 2 below, and quartz glass was obtained in the same procedure as in Test Example 1. In Table 2, the mixing ratio of silica powder and pure water is a mass ratio (weight ratio).
５．試験例１１
平均一次粒子径５０ｎｍのシリカ粉末を用いた。表３に示す混合比でシリカ粉末と純水とを混合して混合物を得た。具体的には、試験例１と同様の攪拌機を用い、まず、常圧での攪拌を５分間行った。次に、３分間の常圧での攪拌と、３分間の真空状態での攪拌とを、連続して行った。攪拌により得られた混合物を、試験例１と同様の手順で成形および加熱処理し、石英ガラスを得た。表３において、シリカ粉末と純水との混合比は、質量比（重量比）である。
5. Test Example 11
Silica powder having an average primary particle diameter of 50 nm was used. Silica powder and pure water were mixed at a mixing ratio shown in Table 3 to obtain a mixture. Specifically, using the same stirrer as in Test Example 1, first, stirring at normal pressure was performed for 5 minutes. Next, stirring at normal pressure for 3 minutes and stirring in a vacuum state for 3 minutes were continuously performed. The mixture obtained by stirring was molded and heat-treated in the same procedure as in Test Example 1 to obtain quartz glass. In Table 3, the mixing ratio of silica powder and pure water is a mass ratio (weight ratio).
［結果］
試験例１０の結果を、表２に示した。表２において、透明な石英ガラスを得られたものを○、成形や透明度に課題があるが石英ガラスが得られたものを△、成形に課題があり石英ガラスを得られなかったものを×として示した。
[result]
The results of Test Example 10 are shown in Table 2. In Table 2, “O” indicates that transparent quartz glass is obtained, “Δ” indicates that there is a problem in molding or transparency, but “Δ” indicates that quartz glass is obtained, and “x” indicates that there is a problem in molding and silica glass cannot be obtained. Indicated.
表２より、平均一次粒子径が７ｎｍ以上４００ｎｍ以下の範囲内で、シリカ粉末と水との混合比を調整することにより、成形が可能な混合物を得ることができ、石英ガラスを製造できた。但し、平均粒子径が１２５ｎｍおよび４００ｎｍのシリカ粉末を用いた場合には、シリカ粉末と水との混合が流動性の良い半透明なスラリーとならず、次の成形工程において注型が困難となったり、混合物が固まりにくく、成形体の表面に剥離が生じたりした。このため、シリカ粉末の平均一次粒子径が７ｎｍ以上１００ｎｍ以下の範囲内であることが好ましいと考えられた。 From Table 2, by adjusting the mixing ratio of silica powder and water within the range of the average primary particle diameter of 7 nm or more and 400 nm or less, a moldable mixture could be obtained, and quartz glass could be produced. However, when silica powder having an average particle size of 125 nm and 400 nm is used, mixing of the silica powder and water does not form a semi-transparent slurry with good fluidity, and casting becomes difficult in the next molding step. Or the mixture was hard to harden, and peeling occurred on the surface of the molded body. For this reason, it was considered that the average primary particle diameter of the silica powder was preferably in the range of 7 nm to 100 nm.
また、平均一次粒子径が７ｎｍ以上５０ｎｍ以下の範囲内で、シリカ粉末と水との混合比を調整することにより、光学部品として用いることのできる、透明な石英ガラスを得られた。 Moreover, transparent quartz glass which can be used as an optical component was obtained by adjusting the mixing ratio of the silica powder and water within the range of the average primary particle diameter of 7 nm or more and 50 nm or less.
また、平均一次粒子径が７ｎｍの場合には、成形工程において混合物を型に注入し、乾燥している間に、亀裂が生じる場合があった。しかし、平均一次粒子径が２２ｎｍ以上５０ｎｍ以下の範囲内では、成形時に亀裂が生じることがなく、良好な成形体を得ることができた。特に、平均一次粒子径が５０ｎｍである場合に、シリカ粉末と水との混合比を適切に調整することで、加熱処理工程における成形体の収縮率を小さくし、所望の形状の石英ガラス（光学部材を含む）を得ることができた。 Further, when the average primary particle diameter is 7 nm, cracks may occur while the mixture is poured into the mold and dried in the molding step. However, when the average primary particle diameter was in the range of 22 nm or more and 50 nm or less, cracks did not occur during molding, and a good molded product could be obtained. In particular, when the average primary particle diameter is 50 nm, by appropriately adjusting the mixing ratio of silica powder and water, the shrinkage ratio of the molded body in the heat treatment step is reduced, and quartz glass (optical Member).
シリカ粉末の平均一次粒子径を５０ｎｍとし、シリカ粉末と水との割合を詳細に検討した試験例１１の結果を、表３に示した。表３において、成形工程における成形性が良好であり、加熱処理工程における収縮率（加熱処理工程により得られた石英ガラス（光学部材）の収縮率）が小さかったものをＡ、成形性や収縮率が中間程度であったものをＢ、成形性や収縮率に難があったものをＣとして示した。 Table 3 shows the results of Test Example 11 in which the average primary particle diameter of the silica powder was 50 nm and the ratio of the silica powder and water was examined in detail. In Table 3, the moldability in the molding process is good, and the shrinkage ratio in the heat treatment process (the shrinkage ratio of the quartz glass (optical member) obtained in the heat treatment process) is A, the moldability and the shrinkage ratio. Was shown as B, and C had difficulty in moldability and shrinkage.
シリカ粉末１０質量部に対する水の混合比が６．１６質量部であった場合に、得られた混合物が、成形工程における型への注入に最も適した粘度となっていた。また、加熱処理工程において収縮率が小さく、成形体の変形が小さかった。シリカ粉末１０質量部に対する水の混合比が６．２１質量部であった場合には、６．１６質量部の場合と比較して、得られた混合物の粘度がやや低く、加熱処理工程において収縮率がやや大きくなった。シリカ粉末１０質量部に対する水の混合比が混合工程完了後６．４質量部であった場合には、得られた混合物の粘度がさらに低く、加熱処理工程において収縮率がさらに大きくなった。シリカ粉末１０質量部に対する水の混合比が６．１５質量部および６．０９であった場合には、６．１６質量部の場合と比較して、得られた混合物の粘度がやや高く、成形工程における型への注入がやや難しくなった。シリカ粉末１０質量部に対する水の混合比が６．０５質量部であった場合には、混合物の粘度が高く、成形工程における型への注入が困難であった。以上より、シリカ粉末の平均一次粒子径を５０ｎｍとした場合に、シリカ粉末１０質量部に対する水の混合比が６．０９質量部以上６．２１質量部以下であることがより好ましく、６．１６質量部であることが最も好ましいと考えられた。 When the mixing ratio of water to 10 parts by mass of silica powder was 6.16 parts by mass, the obtained mixture had a viscosity most suitable for injection into a mold in the molding process. Further, the shrinkage rate was small in the heat treatment step, and the deformation of the molded body was small. When the mixing ratio of water to 10 parts by mass of silica powder is 6.21 parts by mass, the viscosity of the obtained mixture is slightly lower than that of 6.16 parts by mass, and shrinkage occurs in the heat treatment process. The rate has increased slightly. When the mixing ratio of water with respect to 10 parts by mass of silica powder was 6.4 parts by mass after completion of the mixing process, the viscosity of the obtained mixture was further lowered, and the shrinkage rate was further increased in the heat treatment process. When the mixing ratio of water to 10 parts by mass of silica powder was 6.15 parts by mass and 6.09 parts, the viscosity of the obtained mixture was slightly higher than that of 6.16 parts by mass, and molding was performed. Injection into the mold in the process became somewhat difficult. When the mixing ratio of water with respect to 10 parts by mass of silica powder was 6.05 parts by mass, the viscosity of the mixture was high and it was difficult to inject it into the mold in the molding process. From the above, when the average primary particle diameter of the silica powder is 50 nm, the mixing ratio of water to 10 parts by mass of the silica powder is more preferably from 6.09 parts by mass to 6.21 parts by mass, and 6.16. It was thought that it was the most preferable that it was a mass part.
なお、シリカ粉末１０質量部に対する水の混合比が６．０５質量部以上６．４質量部以下の範囲内で、加熱処理工程におけるガラス化には問題がなく、透明な石英ガラスを得ることができた。 In addition, when the mixing ratio of water to 10 parts by mass of silica powder is in the range of 6.05 parts by mass to 6.4 parts by mass, there is no problem in vitrification in the heat treatment step, and transparent quartz glass can be obtained. did it.
真空状態でシリカ粉末と水とを攪拌する工程において、水が蒸発するため、得られた混合物において、シリカ粉末に対する水の含有比は、混合開始時のシリカ粉末に対する水の混合比に比べて小さくなっていた。このため、混合物中のシリカ粉末に対する水の割合を、混合工程完了後の割合で管理することが、より好ましいと考えられた。試験例１１において、混合工程完了後の、混合物中のシリカ粉末に対する水の含有比を表３に示した。表３より、シリカ粉末の平均一次粒子径を５０ｎｍとした場合に、混合工程完了後の、混合物中のシリカ粉末１０重量部に対する水の含有比が５．３２質量部以上５．６７質量部以下であることがより好ましく、５．４１質量部であることが最も好ましいと考えられた。 In the step of stirring the silica powder and water in a vacuum state, water evaporates. Therefore, in the obtained mixture, the content ratio of water to the silica powder is smaller than the mixing ratio of water to the silica powder at the start of mixing. It was. For this reason, it was thought that it was more preferable to manage the ratio of the water with respect to the silica powder in a mixture by the ratio after completion of a mixing process. In Test Example 11, the content ratio of water to the silica powder in the mixture after completion of the mixing step is shown in Table 3. From Table 3, when the average primary particle diameter of the silica powder is 50 nm, the content ratio of water to 10 parts by weight of the silica powder in the mixture after completion of the mixing step is 5.32 parts by mass or more and 5.67 parts by mass or less. It was more preferable, and it was thought that it was the most preferable that it was 5.41 mass parts.
なお、試験例１１では、混合工程が真空状態でシリカ粉末と水とを攪拌する工程を含んでいたが、ある程度減圧された状態でシリカ粉末と水とを混合する工程を含んでいれば、水が蒸発するため、混合物中のシリカ粉末に対する水の割合を、混合工程完了後の割合で管理することが好ましいといえる。 In Test Example 11, the mixing step included a step of stirring the silica powder and water in a vacuum state. However, if the step of mixing the silica powder and water in a state where the pressure was reduced to some extent, Therefore, it can be said that it is preferable to manage the ratio of water to silica powder in the mixture by the ratio after completion of the mixing step.
Claims (12)
前記混合物を成形して成形体を得る成形工程と、
前記成形体を加熱処理して石英ガラスを得る加熱処理工程とを含む、石英ガラスの製造方法。 A mixing step of mixing only silica powder and water to obtain a mixture;
A molding step of molding the mixture to obtain a molded body;
A heat treatment step of heat-treating the molded body to obtain quartz glass.
前記混合工程完了後の前記混合物が、前記水を、前記シリカ粉末１０質量部に対して５．３２質量部以上５．６７質量部以下の割合で含有する、請求項６または請求項７に記載の石英ガラスの製造方法。 The silica powder has an average primary particle size of 50 nm,
The said mixture after completion of the said mixing process contains the said water in the ratio of 5.32 mass parts or more and 5.67 mass parts or less with respect to 10 mass parts of said silica powder. Method for producing quartz glass.
前記第１の昇温速度が、１０℃／ｍｉｎ以上１５℃／ｍｉｎ以下であり、
前記第２の昇温速度が３℃／ｍｉｎである、請求項９に記載の石英ガラスの製造方法。 The predetermined temperature is 900 ° C. or higher and 1000 ° C. or lower,
The first temperature rising rate is 10 ° C./min or more and 15 ° C./min or less,
The manufacturing method of the quartz glass of Claim 9 whose said 2nd temperature increase rate is 3 degrees C / min.
前記成形工程において、前記光学部材の形状に対応する形状を有する型を用いて成形を行う、請求項１から請求項１１のいずれか１項に記載の石英ガラスの製造方法。 The quartz glass is an optical member,
The method for producing quartz glass according to any one of claims 1 to 11, wherein in the molding step, molding is performed using a mold having a shape corresponding to the shape of the optical member.
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