JPH01160843A - Production of neodymium-containing quartz glass - Google Patents
Production of neodymium-containing quartz glassInfo
- Publication number
- JPH01160843A JPH01160843A JP62319238A JP31923887A JPH01160843A JP H01160843 A JPH01160843 A JP H01160843A JP 62319238 A JP62319238 A JP 62319238A JP 31923887 A JP31923887 A JP 31923887A JP H01160843 A JPH01160843 A JP H01160843A
- Authority
- JP
- Japan
- Prior art keywords
- neodymium
- glass
- quartz glass
- added
- gel
- 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.)
- Pending
Links
- 229910052779 Neodymium Inorganic materials 0.000 title claims abstract description 43
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 title claims abstract description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000011521 glass Substances 0.000 claims abstract description 32
- -1 alkyl silicate Chemical compound 0.000 claims abstract description 18
- 150000002798 neodymium compounds Chemical class 0.000 claims abstract description 8
- 238000003980 solgel method Methods 0.000 claims abstract description 7
- 230000002378 acidificating effect Effects 0.000 claims abstract description 6
- 239000010419 fine particle Substances 0.000 claims abstract description 6
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 230000007062 hydrolysis Effects 0.000 claims description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract description 4
- 239000005304 optical glass Substances 0.000 abstract description 3
- 239000010453 quartz Substances 0.000 abstract description 3
- OAGKEKIEPNLLIS-UHFFFAOYSA-N ethanolate neodymium(3+) Chemical compound [Nd+3].CC[O-].CC[O-].CC[O-] OAGKEKIEPNLLIS-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 239000000087 laser glass Substances 0.000 abstract description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 abstract 1
- 238000000034 method Methods 0.000 description 12
- 230000003287 optical effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000002019 doping agent Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 3
- 238000004017 vitrification Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 206010040925 Skin striae Diseases 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002419 bulk glass Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はネオジムを含有した石英ガラスの製造方法に関
する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing quartz glass containing neodymium.
ネオジム含有石英ガラスの製造方法としては、各種の製
法が提案されているが、主に次の３種に大別される。Various manufacturing methods have been proposed as methods for manufacturing neodymium-containing quartz glass, but they are mainly classified into the following three types.
（ａ） 火焔酸化分解溶融法
（ｂ） スート混入ガラス化法 ′
（ｃ） ゾルゲル法
〔発明が解決しようとする問題点〕
しかし、従来の製法では均質で大型のネオジム含有石英
ガラスは得られていない。(a) Flame oxidative decomposition melting method (b) Soot-mixed vitrification method ′ (c) Sol-gel method [Problems to be solved by the invention] However, homogeneous and large neodymium-containing quartz glass cannot be obtained using conventional manufacturing methods. do not have.
火焔酸化分解溶融法及びスート混入ガラス化法では、石
英ガラス中に多量のネオジムを導入することは雑しく、
仮にそれが達成されたとしても脈理の発生は免れない、
また、従来のゾルゲル法は室温程度の液相状態からガラ
スを合成するため、 □ドーパントをガラス中に均一に
導入できるという特長がある反面、大型のガラス体が得
られないという大きな欠点を有していた。したがって、
従来の製造方法では大型で均質性の高いネオジム含有石
英ガラスは非常に得に＜＜、特にネオジムの含有濃度を
増加させようとした場合−層票著となり、実用に供せら
れる材料はほとんど得られないという問題点を有する。In the flame oxidation decomposition melting method and the soot-containing vitrification method, it is cumbersome to introduce a large amount of neodymium into the quartz glass.
Even if this were achieved, the occurrence of striae would not be avoided.
In addition, the conventional sol-gel method synthesizes glass from a liquid phase state at about room temperature, so while it has the advantage of being able to uniformly introduce dopants into the glass, it has the major drawback of not being able to obtain large glass bodies. was. therefore,
With conventional manufacturing methods, large-sized and highly homogeneous neodymium-containing silica glass is extremely difficult to produce.Especially when trying to increase the neodymium concentration, stratification occurs, and very few materials can be used for practical purposes. The problem is that it cannot be used.
そこで本発明の目的とするところは石英レーザーガラス
、光学レンズなどの各種光学部品への応用が可能な十分
高濃度のネオジムを含有しつつ、なおかつ大型で均質な
ネオジム含有石英ガラスの製造方法を提供することにあ
る。Therefore, the purpose of the present invention is to provide a method for manufacturing neodymium-containing quartz glass that is large and homogeneous while containing sufficiently high concentration of neodymium to be applicable to various optical parts such as quartz laser glass and optical lenses. It's about doing.
上記問題点を解決するために、本発明のネオジム含有石
英ガラスの製造方法は、少なくとも以下に示す工程を一
つ以上含むゾルゲル法を用いたガラスの合成において、
アルキルシリケートを酸性触媒により部分加水分解した
後に、ネオジム化合物を少なくとも一種類以上添加する
ことを特徴とする。In order to solve the above problems, the method for producing neodymium-containing quartz glass of the present invention includes at least one or more of the following steps in glass synthesis using a sol-gel method.
The method is characterized in that at least one neodymium compound is added after the alkyl silicate is partially hydrolyzed using an acidic catalyst.
ａ） ネオジム含有加水分解液にシリカ微粒子を分散さ
せる工程。a) A step of dispersing silica fine particles in a neodymium-containing hydrolyzate.
ｂ） シリカ分散液をｐＨ３〜６の範囲に調整する工程
。b) A step of adjusting the pH of the silica dispersion to a range of 3 to 6.
Ｃ） 該ゾル溶液をゲル化、乾燥させドライゲルとする
工程。C) A step of gelling and drying the sol solution to form a dry gel.
ｄ） ドライゲルを熱処理し、ガラス体とする工程。d) A step of heat treating the dry gel to form a glass body.
用いるネオジム化合物としてはアルキルシリケートの部
分加水分解後のゾル溶液に溶解するものであればいずれ
のものでも使用可能である。しかし、アルコキシ化合物
であれば、アルキルシリケートと構造及び反応性が類似
しているため、ネオジム源として理想的である。Any neodymium compound can be used as long as it dissolves in the sol solution after partial hydrolysis of the alkyl silicate. However, alkoxy compounds are ideal as neodymium sources because they are similar in structure and reactivity to alkyl silicates.
前述したように従来のゾルゲル法では、均質性が論じら
れる大きさの塊状ガラス体は得られていない、しかし、
アルキルシリケートの酸性加水分解溶液にシリカ微粒子
を分散させるという製法をとることにより、十分に大き
な塊状のガラス体を容易に得ることが可能である。また
、ゲル化時のｐＨ値を３〜６の範囲に調整することも、
塊状ガラス体を得るうえで極めて大きな効果がある。As mentioned above, in the conventional sol-gel method, it is not possible to obtain a bulk glass body of a size that warrants homogeneity.
By employing a manufacturing method in which fine silica particles are dispersed in an acidic hydrolyzed solution of alkyl silicate, it is possible to easily obtain a sufficiently large glass body in the form of a block. In addition, adjusting the pH value during gelation to a range of 3 to 6 is also possible.
This is extremely effective in obtaining a lumpy glass body.
また、アルキルシリケートを４担部分加水分解した時点
で、ネオジム化合物を添加することにより、ネオジムイ
オンをより効果的にガラスの網目構造中に導入すること
が可能となり、結果として高濃度ドーピングが達成され
やすくなる。この場合のアルキルシリケートの部分加水
分解の程度は、ドーパントの種類、反応性などにより決
定されるが、概ね全加水分解に対し１７６〜５／６の範
囲になる場合が多い。In addition, by adding a neodymium compound when the alkyl silicate is partially hydrolyzed, it becomes possible to more effectively introduce neodymium ions into the network structure of the glass, resulting in high concentration doping. It becomes easier. The degree of partial hydrolysis of the alkyl silicate in this case is determined by the type of dopant, reactivity, etc., but is often in the range of approximately 176 to 5/6 of the total hydrolysis.
以下に本発明の実施例を詳しく述べるが、本発明は以下
の実施例に限定されるものではない。Examples of the present invention will be described in detail below, but the present invention is not limited to the following examples.
〔実施例１〕
エチルシリケート、無水エタノール、水、アンモニア水
（２９％）をモル比で１＝７．６：４二〇。０８の割合
になるように混合し約５時間撹拌した後、室温で数日間
熟成し、減圧濃縮することにより分散性の良いシリカ微
粒子溶液を調製した。[Example 1] Ethyl silicate, absolute ethanol, water, and aqueous ammonia (29%) in a molar ratio of 1=7.6:420. After stirring for about 5 hours, the mixture was aged at room temperature for several days and concentrated under reduced pressure to prepare a silica fine particle solution with good dispersibility.
次にエチルシリケートに同体積量のエタノールとモル比
で１．５倍量の０．２規定塩酸溶液を加え約２時間撹拌
した。その後、ガラス化時にＮｄ／ＳｉＯｔ＝３ｗｔ％
となるように所定量のネオジムをトリエトキシネオジム
なるアルコキシ化合物の形で添加し約１時間撹拌を続け
た。さらに、この溶液にエチルシリケートに対しモル比
で２．５倍量のＯ，Ｏ’２規定の塩酸を加え約１時間撹
拌を行って加水分解溶液を調製した。Next, a 0.2N hydrochloric acid solution of 1.5 times the molar volume as the same volume of ethanol was added to the ethyl silicate and stirred for about 2 hours. After that, during vitrification, Nd/SiOt=3wt%
A predetermined amount of neodymium was added in the form of an alkoxy compound called triethoxyneodymium, and stirring was continued for about 1 hour. Further, to this solution was added O,O'2 normal hydrochloric acid in a molar amount of 2.5 times that of ethyl silicate, and the mixture was stirred for about 1 hour to prepare a hydrolyzed solution.
先に調製したシリカ微粒子溶液のＰＨ値を２規定の塩酸
を用いて４，５に調整した後、ここに加水分解溶液を混
合し、均質な溶液となるまで十分撹拌した。最後にこの
溶液のｐ Ｈを４．８に調整し、室温においてゲル化さ
せた。After adjusting the pH value of the silica fine particle solution prepared previously to 4.5 using 2N hydrochloric acid, the hydrolyzed solution was mixed therein and sufficiently stirred until a homogeneous solution was obtained. Finally, the pH of this solution was adjusted to 4.8 and gelation was performed at room temperature.
このゲル体をポリプロピレン製の乾燥容器（開口率０．
３％程度）に移し入れ、約６０℃に保なれた恒温乾燥機
を用いて約２週間で乾燥し、空気中に放置しても割れな
い多孔質ゲル体を得た。This gel body is dried in a polypropylene drying container (with an opening ratio of 0.
3%) and dried in a constant temperature dryer kept at about 60° C. for about 2 weeks to obtain a porous gel body that does not crack even when left in the air.
このゲル体を酸素／窒素雰囲気中で一旦１００℃まで加
熱し、縮合反応の促進、脱水、親有機物等の各種処理を
行った後、炉内をヘリウム雰囲気に変え、最高１３４０
℃まで加熱してガラス化した。This gel body is heated to 100°C in an oxygen/nitrogen atmosphere and subjected to various treatments such as promotion of condensation reaction, dehydration, and removal of organophilic substances, and then the inside of the furnace is changed to a helium atmosphere.
It was vitrified by heating to ℃.
こうして得られたガラス体は透明性の高い無色のガラス
体で、脈理や結晶化等もみられず良好なもので、その大
きさは１５０＋ｗφＸ５０ｍ＋ｔであり、光学材と用い
るには十分な大きさのものであると言える。もちろん、
この大きさが製造可能なガラス体の上限ではなく、さら
に大きなガラス体も十分製造可能である。また、化学分
析の結果から含有されているネオジム濃度は、Ｎ ｄ
／ Ｓ ｉ Ｏ、＝４．３ｗｔ％であり、仕込み組成と
ほぼ一致していた。The glass body obtained in this way is a colorless glass body with high transparency, and is in good condition with no striae or crystallization.The size of the glass body is 150 + wφ x 50 m + t, which is large enough to be used as an optical material. It can be said that it is a thing. of course,
This size is not the upper limit of the glass body that can be manufactured, and even larger glass bodies can be manufactured. Also, from the results of chemical analysis, the concentration of neodymium contained is N d
/S i O = 4.3 wt%, which was almost the same as the charging composition.
得られたガラス体を１３０ＩＩＩＩφＸ４０ｏｍｔの大
きさに加工し、合わせてその両面を平行平面研磨を行っ
た。ガラス体の各部分での屈折率を詳しく測定し、その
変動幅よりガラス体の均質性を求めたところ、６Ｘ１０
−’以下であった。このガラスは３５０．５８０．７４
０．８００ｎｍなどの特定の波長域で選択的に光吸収を
示すことから、光学フィルターや短波長帯用光学レンズ
として使用できるだけでなく、上記の光吸収帯で光によ
る強励起を行えば、レーザー発振が可能である。実際、
上記ガラス体より６ｆｉφＸ７５ｗＪのロッド状ガラス
体を切り出し、その両端面を高精度平行平面研磨し、レ
ーザー発振を試みたところ、波長１゜０８μｍのレーザ
ー発振を行うことが確認された。The obtained glass body was processed into a size of 130IIIφ×40omt, and both surfaces thereof were polished in parallel planes. The refractive index of each part of the glass body was measured in detail, and the homogeneity of the glass body was determined from the range of variation.
−' or less. This glass is 350.580.74
Since it selectively absorbs light in a specific wavelength range such as 0.800 nm, it can not only be used as an optical filter or an optical lens for short wavelength bands, but also can be used as a laser if intense excitation is performed in the above light absorption band. Oscillation is possible. actual,
A rod-shaped glass body of 6 fi φ x 75 wJ was cut out from the above glass body, both end faces of which were polished into parallel planes with high precision, and when laser oscillation was attempted, it was confirmed that laser oscillation with a wavelength of 1°08 μm was performed.
熱破壊強度の大きい石英をベースにし、そこに発光物質
となるネオジム元素を均一にドーピングしているため、
従来のケイ酸塩系ガラスを用いたレーザーに対して、高
効率、高繰り返し発振が可能であった。It is based on quartz, which has high thermal breakdown strength, and is uniformly doped with neodymium, which becomes a luminescent material.
Compared to conventional lasers using silicate glass, it was possible to oscillate with high efficiency and high repetition rate.
実施例１と同様の方法（本発明の方法；アルキルシリゲ
ートの部分加水分解を行いネオジムのドーピングを行う
方法）と従来の方法（アルキルシリケートの全加水分解
を行った時点でネオジムのドーピングを行う方法）の２
つの製造方法により、ネオジム含有石英ガラスを作製し
、製造方法と得られるガラス体の品質を比較した。尚、
その際、ネオジム濃度（Ｎｄ／５ｉＯ２）を１ｗｔ％、
６ｗｔ％の２種とした。結果を簡略化して第１表に示す
。A method similar to Example 1 (method of the present invention; a method of partially hydrolyzing an alkyl silicate and doping with neodymium) and a conventional method (doping with neodymium after complete hydrolysis of the alkyl silicate) Method) 2
Neodymium-containing quartz glass was manufactured using two manufacturing methods, and the manufacturing methods and quality of the resulting glass bodies were compared. still,
At that time, the neodymium concentration (Nd/5iO2) was 1wt%,
There were two types of 6 wt%. The results are summarized and shown in Table 1.
第１表から、ネオジム濃度が１ｗｔ％の場合には製造方
法と得られるガラス体の品質の間には特に差異は見られ
ないが、ネオジム濃度が６ｗｔ％に増加すると明らかな
差が見られた。つまり、従来法でネオジム濃度が６ｗｔ
％のガラス体を作製した場合、ネオジムイオンが均一に
ガラス網目構造中に導入されず、一部が会合状態をとり
、結果として部分結晶化を生じているものと考えられる
。酸化ネオジムの結晶化については電子顕微鏡及びＥ
ＰＭＡにより容易に確認が可能であった。対して、本発
明の方法ではアルキルシリケートの部分加水分解時にネ
オジムのドーピングを行うため、ドーパントが網目構造
中に入りやすく、結果として均一なドーピングが達成さ
れたものと考えられる。たとえ結晶化の程度が極わずか
であったとしても、光透過性を著しく損なうこととなり
、光学材料として使用するには適当でないと言える４本
比較例から、本発明の製造方法が高濃度のネオジムを含
有する石英ガラスの製法として優れていることがわかる
。尚、本比較例においてはネオジムの含有量として６ｗ
ｔ％という数値を採用したが、これは本発明の製法によ
り導入可能なネオジムの最高量を示すものではない、実
際的には２０数％程度までは導入可能であり、それ以上
の値においても、焼結パラメータの最適化を行うことに
より十分可能であった。Table 1 shows that when the neodymium concentration is 1 wt%, there is no particular difference between the manufacturing method and the quality of the glass body obtained, but when the neodymium concentration increases to 6 wt%, a clear difference is seen. . In other words, with the conventional method, the neodymium concentration was 6wt.
% glass body, neodymium ions are not uniformly introduced into the glass network structure, and some of them assume an associated state, resulting in partial crystallization. For crystallization of neodymium oxide, electron microscopy and E
This could be easily confirmed using PMA. On the other hand, in the method of the present invention, doping with neodymium is performed during partial hydrolysis of the alkyl silicate, so it is thought that the dopant easily enters the network structure, resulting in uniform doping. Even if the degree of crystallization is extremely small, the light transmittance will be significantly impaired and it can be said that it is not suitable for use as an optical material.From the four comparative examples, it is clear that the production method of the present invention is suitable for producing high-concentration neodymium. It can be seen that this is an excellent method for producing quartz glass containing . In addition, in this comparative example, the neodymium content was 6w.
Although the numerical value t% was adopted, this does not indicate the maximum amount of neodymium that can be introduced by the manufacturing method of the present invention; in reality, it is possible to introduce up to about 20%, and even at higher values. This was possible by optimizing the sintering parameters.
第 １ 表
〔発明の効果〕
以上述べたように本発明によれば、少なくとも以下に示
す工程を一つ以上含むゾルゲル法を用いたネオジム含有
石英ガラスの製造方法において、アルキルシリケートを
酸性触媒により部分加水分解した後に、ネオジム化合物
を少なくとも一種類以上添加することにより、多量のネ
オジムをガラス中に均一に導入することが可能となった
。Table 1 [Effects of the Invention] As described above, according to the present invention, in a method for producing neodymium-containing quartz glass using a sol-gel method that includes at least one or more of the following steps, alkyl silicate is partially treated with an acidic catalyst. By adding at least one type of neodymium compound after hydrolysis, it has become possible to uniformly introduce a large amount of neodymium into the glass.
ａ） ネオジム含有加水分解液にシリカ微粒子を分散さ
せる工程。a) A step of dispersing silica fine particles in a neodymium-containing hydrolyzate.
ｂ） シリカ分散液をｐＨ３〜６の範囲に調整する工程
。b) A step of adjusting the pH of the silica dispersion to a range of 3 to 6.
Ｃ） 該ゾル溶液をゲル化、乾燥させドライゲルとする
工程。C) A step of gelling and drying the sol solution to form a dry gel.
ｄ） ドライゲルを熱処理し、ガラス体とする工程。d) A step of heat treating the dry gel to form a glass body.
ネオジム含有石英ガラスは石英ガラスの低膨脹性、高耐
熱性と透れた光透過性に、ネオジムによる選択的光吸収
性と発光性を付加したもので、光学フィルター、光学ガ
ラス、発光ガラス及びレーザーガラス等への広範な応用
が可能なガラスである。この種のガラスを広範な分野で
利用しようとする場合には、ネオジムの含有量を広い範
囲にわたって変化させられることが重要である。しかし
従来の製法ではネオジムの含有量を増大しようとすると
、酸化ネオジムの結晶を生じ透明ガラス体とならないと
いう問題点があったが、本発明の製法を用いることによ
り実用上十分と言える量のネオジムを石英ガラス中に均
一に導入することが可能となり、優れた光学ガラス材と
して広範な応用が可能となったと言える。Neodymium-containing quartz glass combines the low expansion, high heat resistance, and clear light transmission properties of silica glass with the selective light absorption and luminescence properties of neodymium, and is used in optical filters, optical glasses, light-emitting glasses, and lasers. It is a glass that can be used in a wide range of applications such as glass. If this type of glass is to be used in a wide range of fields, it is important to be able to vary the neodymium content over a wide range. However, when trying to increase the neodymium content in the conventional manufacturing method, there was a problem in that neodymium oxide crystals formed and a transparent glass body could not be obtained.However, by using the manufacturing method of the present invention, a practically sufficient amount of neodymium can be uniformly introduced into quartz glass, making it possible to use it in a wide range of applications as an excellent optical glass material.
以上 出願人 セイコーエプソン株式会社that's all Applicant: Seiko Epson Corporation
Claims (2)
ル法を用いたネオジム含有石英ガラスの製造方法におい
て、アルキルシリケートを酸性触媒により部分加水分解
した後に、ネオジム化合物を少なくとも一種類以上添加
することを特徴とするネオジム含有石英ガラスの製造方
法。 ａ）ネオジム含有加水分解液にシリカ微粒子を分散させ
る工程。 ｂ）シリカ分散液をｐＨ３〜６の範囲に調整する工程。 ｃ）該ゾル溶液をゲル化、乾燥させドライゲルとする工
程。 ｄ）ドライゲルを熱処理し、ガラス体とする工程。(1) In a method for producing neodymium-containing quartz glass using a sol-gel method that includes at least one or more of the following steps, at least one neodymium compound may be added after partial hydrolysis of alkyl silicate using an acidic catalyst. A method for producing quartz glass containing neodymium. a) A step of dispersing silica fine particles in a neodymium-containing hydrolyzate. b) A step of adjusting the pH of the silica dispersion to a range of 3 to 6. c) A step of gelling and drying the sol solution to form a dry gel. d) A step of heat treating the dry gel to form a glass body.
特徴とする特許請求の範囲第１項記載のネオジム含有石
英ガラスの製造方法。(2) The method for producing neodymium-containing quartz glass according to claim 1, wherein the neodymium compound is an alkoxy compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62319238A JPH01160843A (en) | 1987-12-17 | 1987-12-17 | Production of neodymium-containing quartz glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62319238A JPH01160843A (en) | 1987-12-17 | 1987-12-17 | Production of neodymium-containing quartz glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01160843A true JPH01160843A (en) | 1989-06-23 |
Family
ID=18107953
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62319238A Pending JPH01160843A (en) | 1987-12-17 | 1987-12-17 | Production of neodymium-containing quartz glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01160843A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1188722A1 (en) * | 2000-08-23 | 2002-03-20 | Heraeus Quarzglas GmbH & Co. KG | Article comprising a body made of quartz glass having improved resistance against plasma corrosion, and method for production thereof |
| SG90270A1 (en) * | 2000-12-22 | 2002-07-23 | Shinetsu Quartz Prod | Quartz glass and quartz glass jig having excellent resistance against plasma corrosion, and method for producing the same |
-
1987
- 1987-12-17 JP JP62319238A patent/JPH01160843A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1188722A1 (en) * | 2000-08-23 | 2002-03-20 | Heraeus Quarzglas GmbH & Co. KG | Article comprising a body made of quartz glass having improved resistance against plasma corrosion, and method for production thereof |
| SG90270A1 (en) * | 2000-12-22 | 2002-07-23 | Shinetsu Quartz Prod | Quartz glass and quartz glass jig having excellent resistance against plasma corrosion, and method for producing the same |
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