JPH02225328A - Production of spherical silica glass - Google Patents
Production of spherical silica glassInfo
- Publication number
- JPH02225328A JPH02225328A JP4394089A JP4394089A JPH02225328A JP H02225328 A JPH02225328 A JP H02225328A JP 4394089 A JP4394089 A JP 4394089A JP 4394089 A JP4394089 A JP 4394089A JP H02225328 A JPH02225328 A JP H02225328A
- Authority
- JP
- Japan
- Prior art keywords
- gel
- acid ester
- silicic acid
- silica glass
- spherical silica
- 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.)
- Granted
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002612 dispersion medium Substances 0.000 claims abstract description 21
- -1 silicic acid ester Chemical class 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 3
- 238000003980 solgel method Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 abstract description 10
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 4
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract description 2
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 60
- 239000002245 particle Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
- 230000003287 optical effect Effects 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 6
- 239000012798 spherical particle Substances 0.000 description 5
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007863 gel particle Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000008096 xylene Substances 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、例えば半導体素子用封止材の充填材（フィシ
）等として使用される球状シリカガラスの製造方法に関
する。更に詳しくはゾル−ゲル法による球状シリカガラ
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 manufacturing spherical silica glass used as a filler (filler) of a sealing material for semiconductor elements, for example. More specifically, the present invention relates to a method for producing spherical silica glass using a sol-gel method.
（従来の技術）
従来、この種の球状シリカガラスの製造方法としては、
天然の珪石および水晶を粉砕し、これを再溶融して球状
化させて球状シリカガラスを製造する方法が知られてい
るが、シリカガラスの高純度化の要求に伴って、これに
代えＳＩＣ！＜１を０２−８２炎中で加水分解してガラ
ススートを作成し、これを温度１８００〜２０００℃で
焼結、粉砕し、再びたび”２ １１２炎中て加熱球状化
させて球状シリカガラスを製造する所謂気相法が採用さ
れてきた。(Prior art) Conventionally, as a method for manufacturing this type of spherical silica glass,
There is a known method of producing spherical silica glass by crushing natural silica stone and crystal, remelting it, and spheroidizing it, but due to the demand for higher purity silica glass, SIC! <1 was hydrolyzed in a 02-82 flame to create a glass soot, which was sintered and crushed at a temperature of 1800 to 2000°C, and then heated again in a 2-112 flame to form a spherical shape to form spherical silica glass. The so-called gas phase method of manufacturing has been adopted.
しかしながら、この気相法は、５ｉＣｊ！、の加水分解
、焼結、粉末の再溶融を温度１８００〜２０００℃の０
２− Ｈ２炎中で行うため、多量の熱エネルギーを必要
とするため、エネルギー費の製造コスト中に占める割合
いが著しく高くなって製品価格は高価であるという問題
がある。However, this gas phase method has 5iCj! , hydrolysis, sintering, and remelting of the powder at a temperature of 1800-2000℃.
Since the process is carried out in a 2-H2 flame, a large amount of thermal energy is required, which causes a problem in that the proportion of energy costs in the manufacturing cost becomes extremely high, making the product expensive.
そこで前記問題点がないものとして特開昭５８−１７６
１３１３号公報に開示されているように珪酸エステル、
水、アルコールの混合溶液を、これらと実質的に相溶性
がない液体に分散、懸濁させて粉粒状のゲルを生成させ
、得られた粉粒状ゲルを分離し焼成させて球状シリカガ
ラスを形成させる所謂ゾル−ゲル法が注目されている。Therefore, assuming that the above-mentioned problem does not exist,
Silicate ester as disclosed in Japanese Patent No. 1313,
A mixed solution of water and alcohol is dispersed and suspended in a liquid that is substantially incompatible with these to form a granular gel, and the resulting granular gel is separated and fired to form spherical silica glass. The so-called sol-gel method is attracting attention.
（発明が解決しようとする課題）
前記ゾル−ゲル法は、生成された粉粒状ゲルの分散に前
記混合溶液と実質的に相溶性がない液体即ち分散媒とし
て、ヘキサノール、オクタツール等の高級アルコール、
ヘキサン、キシレン等の芳香族炭化水素、ジエチルエー
テル、アニソール等のエーテル等を用いているが、生成
したゲル粒子が互いに凝集し易く、完全に単分散した乾
燥ゲルが得られないため、充分に単分散した球状シリカ
ガラスが得られず、また粒径が２ｊＩ１１以上のゲルの
収率が低い等の問題がある。(Problems to be Solved by the Invention) The sol-gel method uses a higher alcohol such as hexanol or octatool as a liquid that is substantially incompatible with the mixed solution, that is, as a dispersion medium, for dispersing the generated powdery gel. ,
Aromatic hydrocarbons such as hexane and xylene, ethers such as diethyl ether and anisole, etc. are used, but the resulting gel particles tend to aggregate with each other, making it impossible to obtain a completely monodispersed dry gel. There are problems in that dispersed spherical silica glass cannot be obtained and the yield of gel having a particle size of 2jI11 or more is low.
本発明は、前記問題点を解消し、ゲルを凝集することな
く良好に分散し得、かつ粒径が２ｊｍ以上のゲルの収率
が良好なゾル−ゲル法による球状シリカガラスの製造方
法を提供することを目的とする。The present invention solves the above-mentioned problems and provides a method for producing spherical silica glass using a sol-gel method, in which the gel can be well dispersed without agglomeration, and the yield of gel having a particle size of 2 jm or more is good. The purpose is to
（課題を解決するための手段）
本発明者らは、前記目的を達成すべく鋭意研究の結果、
ゾル−ゲル法において分散媒に低級アルコールの一つで
あるブタノールを用いると生成されたゲルの分散性が良
好で、かつ粒径２μｍ以上のゲルの収率が向上すること
を知見した。(Means for Solving the Problems) As a result of intensive research to achieve the above object, the present inventors have found that
It has been found that when butanol, which is one of the lower alcohols, is used as a dispersion medium in the sol-gel method, the dispersibility of the generated gel is good and the yield of gel with a particle size of 2 μm or more is improved.
本発明は前記知見に基づいてなされたものであって、そ
の球状シリカガラスの製造方法は、珪酸エステル原料溶
液を加水分解して得られたゾルを分散媒中で分散させて
ゲルを生成させ、得られたゲルを分離、焼成するゾル−
ゲル法により球状シリカガラスを製造する方法において
、前記分散媒としてブタノールを用いることを特徴とす
る。The present invention has been made based on the above findings, and the method for producing spherical silica glass comprises: dispersing a sol obtained by hydrolyzing a silicate ester raw material solution in a dispersion medium to generate a gel; A sol that separates and bakes the resulting gel.
The method for producing spherical silica glass by a gel method is characterized in that butanol is used as the dispersion medium.
本発明で用いる珪酸エステルとしては、珪酸メチル、珪
酸エチル、珪酸プロピル等が挙げられる。Examples of the silicic acid ester used in the present invention include methyl silicate, ethyl silicate, and propyl silicate.
また珪酸エステルの加水分解は、珪酸エステルと、水と
、例えばアンモニア水等の触媒を混合撹拌して懸濁させ
ればよく、その混合比は珪酸エステル１モルに対して水
３〜１０モル＆、 度トし、また触媒としてアンモニア
水を用いる場合は珪酸エステル１モルに対して５ Ｘ
１０−’〜５×１０−３モル程度とするのが好ましい。Hydrolysis of a silicate ester can be carried out by mixing and stirring a silicate ester, water, and a catalyst such as aqueous ammonia, and the mixing ratio is 3 to 10 moles of water to 1 mole of silicate ester. , and when using aqueous ammonia as a catalyst, 5X per mole of silicate ester
The amount is preferably about 10-' to 5 x 10-3 moles.
また、分散媒量は一般には珪酸エステル原料溶液の１〜
３倍容量程度とする。In addition, the amount of dispersion medium is generally 1 to 1 of the silicate ester raw material solution.
It should be about 3 times the capacity.
（実施例） 次に本発明の具体的実施例を比較例と共に説明する。(Example) Next, specific examples of the present invention will be described together with comparative examples.
実験例
先ず、５００ｃｃビーカー中に蒸溜精製した珪酸メチル
１モルに対して蒸溜水５モル、純度９９．５％のアンモ
ニア水１×１０−４モルとなるように夫々加え、マグネ
チックスターラにより温度２５℃で、３０分間激しく撹
拌し、約２５０ｃｃの粘度がｌＯボイズ（東京計器製Ｂ
型粘度計）のゾルを調製した。Experimental Example First, 5 moles of distilled water and 1 x 10-4 moles of ammonia water with a purity of 99.5% were added to 1 mole of methyl silicate purified by distillation into a 500cc beaker, and the mixture was heated to 25% using a magnetic stirrer. ℃, stirred vigorously for 30 minutes, and a viscosity of about 250 cc was obtained using 1O bois (Tokyo Keiki B).
(type viscometer) was prepared.
次に、前記ゾルｚｓｏｃｃを、別個に用意した１０００
ｃｃビーカー中の前記ゾル量に対して容積比で２倍容量
のブタノール分散液中に投入し、マグネチックスターラ
によって温度２５℃で、５時間激しく撹拌して、ゲルを
生成させた。Next, the sol zsocc was prepared separately.
The mixture was poured into a butanol dispersion having a volume ratio twice that of the sol in the CC beaker, and vigorously stirred with a magnetic stirrer at a temperature of 25° C. for 5 hours to form a gel.
撹拌終了後直ちに静置させて生成されたゲルの沈降開始
時間と、静置５分経過後のゲルの分散状態を調べ、その
結果を表に示した。Immediately after the stirring was completed, the gel was allowed to stand still, and the sedimentation start time and the dispersion state of the gel after 5 minutes of standing were investigated, and the results are shown in the table.
また生成されたゲルを光学顕微鏡で観察（倍率１００倍
）したところ粒径が２〜１００μｍ程度の球状粒子とし
て単分散していることが確認された。Further, when the produced gel was observed with an optical microscope (magnification: 100 times), it was confirmed that it was monodispersed as spherical particles with a particle size of about 2 to 100 μm.
次いで生成されたゲル分散液を孔径が２：ｌｌ１１の濾
紙を用いて減圧濾過してゲルと濾液に分離し、濾紙上の
ゲルを純度９８％のブタノール５００ｃｃで２回、次い
で蒸溜水２５０ｃｃで１回洗浄後、温度ＢＯ℃、湿度９
５％の恒温恒湿器内で２４時間乾燥した。Next, the generated gel dispersion was filtered under reduced pressure using a filter paper with a pore size of 2:111 to separate the gel and the filtrate. After washing twice, temperature BO℃, humidity 9
It was dried for 24 hours in a 5% temperature and humidity chamber.
乾燥後の粒状ゲルを電気炉内で昇温速度１００”Ｃ／１
時間で温度８００℃まで昇温し、該温度で２時間焼成し
たのち、常温まで冷却して球状シリカガラスを得た。After drying, the granular gel is heated at a heating rate of 100”C/1 in an electric furnace.
The temperature was raised to 800° C. for 2 hours, and after firing at this temperature for 2 hours, it was cooled to room temperature to obtain spherical silica glass.
得られた白色粉末をＸ線回折法で調べたところシリカガ
ラスであることが確認された。When the obtained white powder was examined by X-ray diffraction, it was confirmed that it was silica glass.
また、得られたゲルの収率を次式により求め、その結果
を表に示した。Further, the yield of the obtained gel was determined using the following formula, and the results are shown in the table.
尚、ＭＸ：得られた球状シリカガラス量。Incidentally, MX: amount of obtained spherical silica glass.
ＭＡ：原料に用いた珪酸メチル量から理論的に計算され
るシリカガラス量。MA: The amount of silica glass theoretically calculated from the amount of methyl silicate used in the raw material.
比較実験例１
ゾルを分散させる分散媒にブタノールの代わりにプロパ
ツールを用いた以外は実験例と同様の方法で球状シリカ
ガラスを作成した。Comparative Experimental Example 1 Spherical silica glass was produced in the same manner as in the experimental example except that propatool was used instead of butanol as the dispersion medium for dispersing the sol.
前記実験例と同様にして、撹拌後直ちに静置させて生成
されたゲルの沈降開始時間と、静置５分経過後のゲルの
分散状態並びにゲルの収率を調べ、その結果を表に示し
た。In the same manner as in the above experimental example, the settling start time of the gel produced by allowing it to stand immediately after stirring, the dispersion state of the gel after 5 minutes of standing, and the gel yield were investigated, and the results are shown in the table. Ta.
また、生成されたゲルを光学顕微鏡で観察（倍率１００
０倍）したところ粒径が１νｍ以下の均一な球状粒子と
して単分散していた。In addition, the generated gel was observed under an optical microscope (magnification: 100
0 times), it was found that the particles were monodispersed as uniform spherical particles with a particle size of 1 νm or less.
比較実験例２
ゾルを分散させる分散媒にブタノールの代わりにヘキサ
ノールを用いた以外は実施例と同様の方法で球状シリカ
ガラスを作成した。Comparative Experimental Example 2 Spherical silica glass was produced in the same manner as in Example except that hexanol was used instead of butanol as the dispersion medium for dispersing the sol.
前記実験例と同様にして、撹拌後直ちに静置させて生成
されたゲルの沈降開始時間と、静置５分経過後のゲルの
分散状態並びにゲルの収率を調べ、その結果を表に示し
た。In the same manner as in the above experimental example, the settling start time of the gel produced by allowing it to stand immediately after stirring, the dispersion state of the gel after 5 minutes of standing, and the gel yield were investigated, and the results are shown in the table. Ta.
また、生成されたゲルを光学顕微鏡で観察（倍率１００
倍）したところ粒径が２〜１００μｍの球状粒子が複数
個凝集していた。In addition, the generated gel was observed under an optical microscope (magnification: 100
As a result, a plurality of spherical particles having a particle size of 2 to 100 μm were aggregated.
比較実験例３
ゾルを分散させる分散媒にブタノールの代わりにヘプタ
ツールを用いた以外は実験例と同様の方法で球状シリカ
ガラスを作成した。Comparative Experimental Example 3 Spherical silica glass was produced in the same manner as in Experimental Example except that heptatool was used instead of butanol as the dispersion medium for dispersing the sol.
前記実験例と同様にして、撹拌後直ちに静置させて生成
されたゲルの沈降開始時間と、静置５分経過後のゲルの
分散状態並びにゲルの収率を調べ、その結果を表に示し
た。In the same manner as in the above experimental example, the settling start time of the gel produced by allowing it to stand immediately after stirring, the dispersion state of the gel after 5 minutes of standing, and the gel yield were investigated, and the results are shown in the table. Ta.
また、生成されたゲルを光学顕微鏡で観察（倍率１００
倍）したところ粒径が２〜１００μｍの球状粒子が複数
個凝集していた。In addition, the generated gel was observed under an optical microscope (magnification: 100
As a result, a plurality of spherical particles having a particle size of 2 to 100 μm were aggregated.
比較実験例４
ゾルを分散させる分散媒にブタノールの代わりにオクタ
ツールを用いた以外は実験例と同様の方法で球状シリカ
ガラスを作成した。Comparative Experimental Example 4 Spherical silica glass was produced in the same manner as in Experimental Example except that octatool was used instead of butanol as the dispersion medium for dispersing the sol.
前記実験例と同様にして、撹拌後直ちに静置させて生成
されたゲルの沈降開始時間と、静置５分経過後のゲルの
分散状態並びにゲルの収率を調べ、その結果を表に示し
た。In the same manner as in the above experimental example, the settling start time of the gel produced by allowing it to stand immediately after stirring, the dispersion state of the gel after 5 minutes of standing, and the gel yield were investigated, and the results are shown in the table. Ta.
また、生成されたゲルを光学顕微鏡で観察（倍率１００
倍）したところ粒径が２〜ｉｏｏ ａｍの球状粒子が複
数個凝集していた。In addition, the generated gel was observed under an optical microscope (magnification: 100
As a result, a plurality of spherical particles having a particle size of 2 to 100 am were aggregated.
比較実験例５
ゾルを分散させる分散媒にブタノールの代わりにヘキサ
ンを用いた以外は実験例と同様の方法で球状シリカガラ
スを作成した。Comparative Experimental Example 5 Spherical silica glass was produced in the same manner as in Experimental Example except that hexane was used instead of butanol as the dispersion medium for dispersing the sol.
前記実験例と同様にして、撹拌後直ちに静置させて生成
されたゲルの沈降開始時間と、静置５分経過後のゲルの
分散状態並びにゲルの収率を調べ、その結果を表に示し
た。In the same manner as in the above experimental example, the settling start time of the gel produced by allowing it to stand immediately after stirring, the dispersion state of the gel after 5 minutes of standing, and the gel yield were investigated, and the results are shown in the table. Ta.
また、生成されたゲルを光学顕微鏡で観察（倍率１００
倍）したところ粒径がｌＯ〜２００１ｍの塊状粒子が生
成していた。In addition, the generated gel was observed under an optical microscope (magnification: 100
As a result, it was found that lumpy particles with a particle size of 10 to 2001 m were produced.
比較実験例６
ゾルを分散させる分散媒にブタノールの代わりにヘプタ
ンを用いた以外は実験例と同様の方法で球状シリカガラ
スを作成した。Comparative Experimental Example 6 Spherical silica glass was produced in the same manner as in Experimental Example except that heptane was used instead of butanol as the dispersion medium for dispersing the sol.
前記実験例と同様にして、撹拌後直ちに静置させて生成
されたゲルの沈降開始時間と、静置５分経過後のゲルの
分散状態並びにゲルの収率を調べ、その結果を表に示し
た。In the same manner as in the above experimental example, the settling start time of the gel produced by allowing it to stand immediately after stirring, the dispersion state of the gel after 5 minutes of standing, and the gel yield were investigated, and the results are shown in the table. Ta.
また、生成されたゲルを光学顕微鏡で観察（倍率１００
倍）したところ粒径が１０〜２００μｍの塊状粒子が生
成していた。In addition, the generated gel was observed under an optical microscope (magnification: 100
As a result, bulk particles with a particle size of 10 to 200 μm were produced.
比較実験例７
ゾルを分散させる分散媒にブタノールの代わりにトルエ
ンを用いた以外は実験例と同様の方法で球状シリカガラ
スを作成した。Comparative Experimental Example 7 Spherical silica glass was produced in the same manner as in Experimental Example except that toluene was used instead of butanol as the dispersion medium for dispersing the sol.
前記実験例と同様にして、撹拌後直ちに静置させて生成
されたゲルの沈降開始時間と、静置５分経過後のゲルの
分散状態並びにゲルの収率を調べ、その結果を表に示し
た。In the same manner as in the above experimental example, the settling start time of the gel produced by allowing it to stand immediately after stirring, the dispersion state of the gel after 5 minutes of standing, and the gel yield were investigated, and the results are shown in the table. Ta.
また、生成されたゲルを光学顕微鏡で観察（倍率１００
倍）したところ粒径が１０〜２００μｍの塊状粒子が生
成していた。In addition, the generated gel was observed under an optical microscope (magnification: 100
As a result, bulk particles with a particle size of 10 to 200 μm were produced.
表 尚、表におけるゲルの分散性の評価は次の通りである。table In addition, the evaluation of the dispersibility of the gel in the table is as follows.
◎ 分散性極めて良好
Ｏ分散性良好
△ 凝集状態
× 凝集状態が著しい
表から明らかなように、分散媒にブタノールを用いた本
発明の実験例の方法は、ゲルの分散性が良好であり、か
つ粒径２μｍ以上のゲルの収率も高かった。これに対し
て分散媒にプロパツールを用いた比較実験例１の方法は
、ゲルの分散性は良好であるがゲルの沈降開始が遅く、
かつ生成されたゲルの粒径が極めて小さいため粒径２ｐ
ｍ以上のゲル収率が０であった。また分散媒にヘキサノ
ール、ヘプタツール、オクタツール等の高級アルコール
を用いた比較実験例２〜４の方法は、ゲルの沈降開始は
非常に速くゲルの分散性が悪く、かつゲルの収率が低か
った。◎ Very good dispersibility O Good dispersibility △ Agglomerated state The yield of gels with particle sizes of 2 μm or more was also high. On the other hand, in the method of Comparative Experiment Example 1 using propatool as the dispersion medium, the dispersibility of the gel was good, but the gel began to settle slowly.
And the particle size of the generated gel is extremely small, so the particle size is 2p.
The gel yield of m or more was 0. In addition, in the methods of Comparative Experiments 2 to 4 in which higher alcohols such as hexanol, heptatool, and octatool were used as the dispersion medium, the gel sedimentation started very quickly, the gel dispersibility was poor, and the gel yield was low. Ta.
また分散媒にヘキサン、ヘプタン、トルエンを用いた比
較実験例５〜７の方法では、ゲルは分散せずに塊状であ
った。Furthermore, in the methods of Comparative Experiments 5 to 7 in which hexane, heptane, or toluene was used as the dispersion medium, the gels were not dispersed but were in the form of lumps.
（発明の効果）
このように球状シリカガラスの製造方法によれば、分散
媒としてブタノールを用いるようにしたので、生成され
たゲルが凝集することなく均一に分散媒中に分散し、か
つ粒径２１ｍ以上のゲルの収率を向上させることが出来
、分散性のよい球状シリカガラスを高収率で製造出来る
等の効果を１−ｆする。(Effects of the Invention) According to the method for producing spherical silica glass, butanol is used as the dispersion medium, so that the generated gel is uniformly dispersed in the dispersion medium without agglomeration, and the particle size Effects such as being able to improve the yield of gels of 21 m or more and producing spherical silica glass with good dispersibility at a high yield are 1-f.
特 許 出 願 人 日本無機株式会社 外３名 平成 年 月 日Patent applicant Nihon Muki Co., Ltd. 3 other people Month, Heisei Day
Claims (1)
散媒中で分散させてゲルを生成させ、得られたゲルを分
離、焼成するゾル−ゲル法により球状シリカガラスを製
造する方法において、前記分散媒としてブタノールを用
いることを特徴とする球状シリカガラスの製造方法。In the method for producing spherical silica glass by the sol-gel method, the sol obtained by hydrolyzing a silicate ester raw material solution is dispersed in a dispersion medium to form a gel, and the resulting gel is separated and fired. A method for producing spherical silica glass characterized by using butanol as a dispersion medium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4394089A JPH02225328A (en) | 1989-02-23 | 1989-02-23 | Production of spherical silica glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4394089A JPH02225328A (en) | 1989-02-23 | 1989-02-23 | Production of spherical silica glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02225328A true JPH02225328A (en) | 1990-09-07 |
| JPH0519494B2 JPH0519494B2 (en) | 1993-03-16 |
Family
ID=12677698
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4394089A Granted JPH02225328A (en) | 1989-02-23 | 1989-02-23 | Production of spherical silica glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02225328A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4225978C1 (en) * | 1992-08-06 | 1994-04-07 | Degussa | Shaped organosiloxane polycondensates, process for their preparation and use |
| JP2016539903A (en) * | 2013-11-26 | 2016-12-22 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングＭｅｒｃｋ Ｐａｔｅｎｔ Ｇｅｓｅｌｌｓｃｈａｆｔ ｍｉｔ ｂｅｓｃｈｒａｅｎｋｔｅｒ Ｈａｆｔｕｎｇ | Process for producing inorganic particulate material |
-
1989
- 1989-02-23 JP JP4394089A patent/JPH02225328A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4225978C1 (en) * | 1992-08-06 | 1994-04-07 | Degussa | Shaped organosiloxane polycondensates, process for their preparation and use |
| JP2016539903A (en) * | 2013-11-26 | 2016-12-22 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングＭｅｒｃｋ Ｐａｔｅｎｔ Ｇｅｓｅｌｌｓｃｈａｆｔ ｍｉｔ ｂｅｓｃｈｒａｅｎｋｔｅｒ Ｈａｆｔｕｎｇ | Process for producing inorganic particulate material |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0519494B2 (en) | 1993-03-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zawrah et al. | Facile and economic synthesis of silica nanoparticles | |
| JPH02503790A (en) | sinterable nitride | |
| JPS61201623A (en) | Production of spherical flocculated particle of zirconia ultrafine crystal | |
| EP0331187B1 (en) | Process for producing a ceramic preform | |
| JPH02225328A (en) | Production of spherical silica glass | |
| JPH085660B2 (en) | Method for producing silica gel containing titanium oxide ultrafine particles dispersed therein | |
| KR960003236B1 (en) | Method for preparing silica gel particles | |
| JPS5939366B2 (en) | Manufacturing method of zirconium oxide fine powder | |
| JPS6197134A (en) | Powder of zirconia agglomerated particle and preparation thereof | |
| JPH02307830A (en) | Production of quartz glass powder | |
| US4774068A (en) | Method for production of mullite of high purity | |
| JP2903242B2 (en) | Method for producing powdery spherical silica glass | |
| JPS62158116A (en) | Production of fine aluminium oxide particles | |
| JPS61204033A (en) | Granulating method for powder of inorganic raw material | |
| JPH02293314A (en) | Aggregate of particle and production thereof | |
| JP2010254574A (en) | Spherical multicomponent glass fine particle | |
| JP4822550B2 (en) | Spherical multi-component glass particles | |
| RU2144505C1 (en) | Method of preparing titanium dioxide | |
| JPH02184514A (en) | Cylindrical quartz glass powder and production thereof | |
| JP2734083B2 (en) | Method for producing transparent quartz glass molded body | |
| JPS62226821A (en) | Production of glass | |
| CN1049485A (en) | The production method of the compound material of metal oxide, metal oxide composite material powder end and stupalith | |
| JPH0521855B2 (en) | ||
| CN1375457A (en) | Prepn. of nano yttrium oxide | |
| JPH02225327A (en) | Production of filler for sealing material and hollow spherical silica glass |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313113 |
|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| LAPS | Cancellation because of no payment of annual fees |