JPH02225327A - Production of filler for sealing material and hollow spherical silica glass - Google Patents
Production of filler for sealing material and hollow spherical silica glassInfo
- Publication number
- JPH02225327A JPH02225327A JP4393989A JP4393989A JPH02225327A JP H02225327 A JPH02225327 A JP H02225327A JP 4393989 A JP4393989 A JP 4393989A JP 4393989 A JP4393989 A JP 4393989A JP H02225327 A JPH02225327 A JP H02225327A
- Authority
- JP
- Japan
- Prior art keywords
- gel
- spherical silica
- hollow
- temperature
- silica glass
- 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 53
- 239000000945 filler Substances 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000003566 sealing material Substances 0.000 title abstract description 10
- 239000002612 dispersion medium Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- -1 silicic acid ester Chemical class 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 32
- 238000010304 firing Methods 0.000 claims description 7
- 239000000565 sealant Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 10
- 239000007787 solid Substances 0.000 abstract description 9
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 3
- 230000020169 heat generation Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 230000003111 delayed effect Effects 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 26
- 239000011240 wet gel Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000008393 encapsulating agent Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000007863 gel particle Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/107—Forming hollow beads
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、半導体素子用封止材の充填材（フィシ）とし
て使用するのに適した中空球状シリカガラスおよびその
製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a hollow spherical silica glass suitable for use as a filler in a sealing material for semiconductor devices, and a method for manufacturing the same.
（従来の技術）
従来、この種の充填材としては半導体素子の放熱を助け
、更に熱サイクルによる応力を低減させるために、熱伝
導度が大きく、熱膨張係数が小さいこと、その他機械的
強度の点から球状シリカガラスが用いられているが、半
導体素子をコンピューター等の高周波域で使用する際に
生じる発熱をより低減することが出来る封止材用充填材
の提案が望まれていた。(Prior art) Conventionally, this type of filler has been used to help heat dissipation from semiconductor devices and to reduce stress caused by thermal cycles. Although spherical silica glass has been used for this reason, it has been desired to propose a filler for encapsulants that can further reduce the heat generated when semiconductor elements are used in high frequency ranges such as computers.
（発明が解決しようとする課題）
本発明は、前記要望を満たす封止材用充填材および該充
填材として使用される中空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。(Problems to be Solved by the Invention) An object of the present invention is to provide a filler for a sealant that satisfies the above-mentioned needs and a method for producing hollow spherical silica glass used as the filler.
（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、
従来の中実球状シリカガラス（中身が充填された球状シ
リカガラス）を中空にすることによって前記要望を満た
す封止材用充填材が得られることを知見した。(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 by making conventional solid spherical silica glass (filled spherical silica glass) hollow, it is possible to obtain a filler for an encapsulant that satisfies the above requirements.
本発明は前記知見に基づいてなされたものであって、そ
の封止材用充填材は、粒径が従来の中実球状シリカガラ
スの粒径と同程度の中空球状シリカガラスである。。The present invention has been made based on the above findings, and the filler for the sealing material is hollow spherical silica glass having a particle size comparable to that of conventional solid spherical silica glass. .
また、中空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し、湿度
５０２６以上、温度４０〜９０℃の条件下で乾燥させた
後、焼成することを特徴とする。In addition, the method for manufacturing hollow spherical silica glass involves dispersing a sol obtained by hydrolyzing a silicate ester raw material solution in a dispersion medium to generate a gel, separating the resulting gel, and then controlling the temperature at a humidity of 5026 or higher and at a temperature of It is characterized in that it is dried under conditions of 40 to 90°C and then fired.
本発明の製造方法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 production method of the present invention include methyl silicate, ethyl silicate, propyl silicate, and the like.
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モル程度とし、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
−’〜５Ｘ１０−’モル程度とするのが好ましい。Hydrolysis of silicate ester can be carried out by mixing and stirring silicate ester, water, and a catalyst such as aqueous ammonia, and the mixing ratio is about 3 to 10 moles of water to 1 mole of silicate ester. and when using aqueous ammonia as a catalyst, 5 x 10 per mole of silicate ester.
-' to about 5×10-' moles is preferable.
また、本発明の製造方法で用いる分散媒としては、原料
溶液と相溶性がないか或いは極めて小さい液体であれば
よく、例えばブタノール、ヘキサノール、オクタツール
、トルエンが挙げられる。Further, the dispersion medium used in the production method of the present invention may be any liquid that is incompatible with the raw material solution or has a very small size, and examples thereof include butanol, hexanol, octatool, and toluene.
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.
また生成、分離されたゲルに施す乾燥を湿度５０％以上
、温度４０〜９０℃としたのは、乾燥速度が速すぎる場
合には粒状ゲルの中空形成が早く行われて中空ゲルの皮
が肉薄になって中空ゲルの皮が破損しやすく、また乾燥
速度が遅すぎる場合には粒状ゲルの中空形成が遅くなっ
て皮が肉厚の粒状ゲル或いは中実の粒状ゲルしか得られ
ず封止材用充填材に適する中空球状シリカガラスが得ら
れない等の理由からである。Furthermore, the reason why the produced and separated gel was dried at a humidity of 50% or more and a temperature of 40 to 90°C is because if the drying speed is too fast, the formation of hollow particles in the granular gel occurs quickly, resulting in a thin shell of the hollow gel. If the drying speed is too slow, the formation of hollow gel in the granular gel will be slow and only a granular gel with a thick skin or a solid granular gel will be obtained and the sealing material will be damaged. This is because hollow spherical silica glass suitable for use as a filler cannot be obtained.
乾燥後の焼成については、例えば、前記焼成を温度９０
０℃以下で熱処理した後、更に温度１０００〜１７００
℃で浮遊状態で熱処理を行うようにすれば良好な中空球
状シリカガラスが得られる。Regarding the firing after drying, for example, the firing is performed at a temperature of 90°C.
After heat treatment at 0°C or lower, further heat treatment at a temperature of 1000 to 1700°C
If heat treatment is performed in a floating state at ℃, good hollow spherical silica glass can be obtained.
尚、温度９００℃以下での熱処理は所望温度までの温度
上昇速度は出来る限り緩やかに行う方がゲル粒子を発泡
或いは破裂させることなく乾燥状態のままシリカを充分
にガラス化させるのに好都合であり、該温度上昇速度は
一般には１００℃／１時間程度とする。It should be noted that in heat treatment at a temperature of 900° C. or lower, it is better to perform the temperature increase rate as slowly as possible to the desired temperature in order to sufficiently vitrify the silica in a dry state without causing foaming or bursting of the gel particles. The rate of temperature increase is generally about 100° C./hour.
また、温度１ｏｏｏ〜１７００℃で浮遊状態での熱処理
はゲル粉体を例えば電気炉内に該炉の一方より送り込ん
で浮遊状態で熱処理した後、該炉の他方から回収するよ
うにすればよい。尚、ゲル粉体を浮遊状態でなく静止状
態で熱処理を施した場合は球状シリカガラス同士が摩管
し易くなり、また皮のガラス質が緻密でかつ所定厚さの
中空球状シリカガラスが得られなくなるので好ましくな
い。Further, the heat treatment in a floating state at a temperature of 100 to 1700° C. may be carried out by feeding the gel powder into an electric furnace from one side of the furnace, heat-treating it in a floating state, and then recovering it from the other side of the furnace. In addition, if the gel powder is heat-treated in a static state rather than in a floating state, the spherical silica glasses will easily rub together, and a hollow spherical silica glass with a dense glassy skin and a predetermined thickness will be obtained. I don't like it because it disappears.
（実施例）
次に本発明の封止材用充填材並びに中空球状シリカガラ
スの製造方法の具体的実施例を比較例と共に説明する。(Example) Next, specific examples of the manufacturing method of the filler for sealing material and hollow spherical silica glass of the present invention will be described together with comparative examples.
実施例
先ず、５００ｃｃの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×ｌＯ″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１０分間激しく撹
拌し、約２５０ｃｃの粘度が１０ボイズ（東京計器製Ｂ
型粘度計）のゾルを調整した。Example First, 5 moles of distilled water and 4 moles of 99.5% pure ammonia water were added to 1 mole of distilled methyl silicate in a 500 cc beaker, and the temperature was adjusted using a magnetic stirrer. Stir vigorously for 10 minutes at 25°C until the viscosity of approximately 250 cc is 10 voices (Tokyo Keiki B).
(type viscometer) was adjusted.
次に、前記ゾル２５０ｃｃ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
の純度９８％のブタノールから成る分散媒中に投入し、
マグネチックスターラにより温度２５℃で、５時間激し
く撹拌して、ウェットゲルを生成させた。生成されたウ
ェットゲルは分散媒中で白濁浮遊していた。Next, 250 cc of the sol was added to a separately prepared 1000 ml
Pour into a dispersion medium consisting of butanol with a purity of 98%, which is twice the volume of the sol in the cc beaker,
The mixture was vigorously stirred with a magnetic stirrer at a temperature of 25° C. for 5 hours to form a wet gel. The produced wet gel was cloudy and suspended in the dispersion medium.
続いて生成されたウェットゲル分散媒液を孔径が３．Ｈ
の濾紙を用いて減圧濾過してウェットゲルと濾液に分離
し、濾紙上のウェットゲルを純度９８％のブタノール５
００ｃｃで２回、次いで蒸溜水３００ｃｃで１回洗浄し
た。Subsequently, the produced wet gel dispersion medium was mixed with a pore size of 3. H
The wet gel and filtrate are separated by vacuum filtration using a filter paper of
It was washed twice with 00 cc of water and then once with 300 cc of distilled water.
洗浄後のウェットゲルを透過型顕微鏡（倍率１００倍）
で観察したところ粒径が５〜８０Ｉ１ｍの透明なゲルで
あった。Transmission microscope (100x magnification) of wet gel after washing
When observed, it was found to be a transparent gel with a particle size of 5 to 80 lm.
次いで前記方法でゲル分散媒液中から分離されたウェッ
トゲルを恒温恒湿器内で湿度４０％。Next, the wet gel separated from the gel dispersion medium in the above method was kept at a humidity of 40% in a constant temperature and humidity chamber.
５０％、６０％、 ７０９６．８０％、９０％、９５％
の各条件下で、温度を２５℃、４０℃、８０’Ｃ１８０
℃、９０℃、１００℃として２４時間乾燥した。50%, 60%, 7096.80%, 90%, 95%
Under each condition of 25℃, 40℃, 80'C180
℃, 90℃, and 100℃ for 24 hours.
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℃まで昇温した後、該温度で２時間焼
成して粒径３〜６０ｊｍの球状シリカを作成した。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. over an hour, and then fired at this temperature for 2 hours to produce spherical silica having a particle size of 3 to 60 μm.
作成された夫々の球状シリカを透過型顕微鏡（倍率２０
０倍）で粒子の空洞状態を調べ、その結果を表に示した
。Each created spherical silica was examined under a transmission microscope (magnification: 20
The hollow state of the particles was examined under magnification (0x), and the results are shown in the table.
表
尚、表における符号は球状シリカの空洞状態の大きさを
示すものである。Table Note that the symbols in the table indicate the size of the hollow state of the spherical silica.
Ａ・・・空洞部分が大きい
Ｂ・・・空洞部分が普通
Ｃ・・・空洞部分が小さい
Ｄ・・・内部に空洞部分なし
く中実球状体）
表から明らかなように分散媒より分離されたゲルを乾燥
させる際、湿度が低く温度が高い程球状シリカの空洞部
分は大きく、湿度が高く温度が低い程球状シリカの空洞
部分が小さくなって中実球状体に近づく。従って分散媒
より分離されたゲルの乾燥条件は湿度５０％以上、温度
４０〜９０℃で行うことが最適であることが確認された
。A: Large cavity B: Normal cavity C: Small cavity D: Solid spherical body with no internal cavity) As is clear from the table, it is separated from the dispersion medium. When drying the gel, the lower the humidity and the higher the temperature, the larger the hollow part of the spherical silica becomes, and the higher the humidity and lower the temperature, the smaller the hollow part of the spherical silica becomes, approaching a solid spherical body. Therefore, it was confirmed that the optimum conditions for drying the gel separated from the dispersion medium are a humidity of 50% or more and a temperature of 40 to 90°C.
次に、前記方法のうちでウェットゲルの乾燥を湿度９０
％、温度６０℃とし、乾燥後温度８００℃の熱処理を施
して得られた球状シリカを内径１０印、長さ２００ｃｍ
とした縦型電気炉内に配設された内径８ｃｍ、長さ１５
０印のアイレミナ材から成る耐熱性加熱管内に該加熱管
の下部から１００ｇ／１分間の速度で空気と共に送り込
み、浮遊状態で数秒間の熱処理を施した後、加熱管の上
部から中空球状シリカガラスから成る封止材用充填材を
回収した。尚、加熱管による熱処理温度は１００℃単位
で９００℃から１８００℃とした。Next, in the above method, dry the wet gel at a humidity of 90%.
%, the temperature was 60℃, and after drying, the spherical silica obtained by heat treatment at a temperature of 800℃ had an inner diameter of 10 marks and a length of 200cm.
An inner diameter of 8 cm and a length of 15 cm was installed in a vertical electric furnace.
Air is fed into a heat-resistant heating tube made of 0-marked Airemina material from the bottom of the heating tube at a rate of 100 g/minute, and after heat treatment for several seconds in a floating state, hollow spherical silica glass is poured from the top of the heating tube. A filler for sealing material consisting of was collected. The heat treatment temperature using the heating tube was 900°C to 1800°C in 100°C increments.
得られた中空球状シリカガラスから成る封止材用充填材
の空洞状態と、ガラス質について調べたところ、熱処理
温度が１０００〜１７００℃では得られた中空球状シリ
カガラスは中空のままでガラス質の緻密化が進行してお
り、またシリカガラスは透明であった。しかし熱処理温
度が１８００℃以上では得られた球状シリカガラスは空
洞部分が維持されずに中実状態であった。また熱処理温
度が９００℃以下では得られた球状シリカガラスは緻密
化が進行しておらず、多孔質であった。When we investigated the hollow state and glass quality of the obtained filler for sealing material made of hollow spherical silica glass, we found that when the heat treatment temperature was 1000 to 1700°C, the obtained hollow spherical silica glass remained hollow and became glassy. Densification was progressing, and the silica glass was transparent. However, when the heat treatment temperature was 1800° C. or higher, the resulting spherical silica glass did not maintain its hollow portion and remained solid. Further, when the heat treatment temperature was 900° C. or lower, the obtained spherical silica glass did not become densified and was porous.
比較例
ウェットゲルの乾燥を湿度９０％、温度６０℃とした以
外は前記実施例と同様の方法で乾燥ゲルを作成した。Comparative Example A dry gel was prepared in the same manner as in the previous example except that the wet gel was dried at a humidity of 90% and a temperature of 60°C.
作成された乾燥ゲルに温度８００℃の熱処理を行うこと
なく該ゲルを直接内径１０ｃ＋＋＋、長さ２００１とし
た縦型電気炉内に配設された内径８ＣＩＴ１％長さ１５
０ ｃｍのアルミナ材から成る耐熱性加熱管内に該加熱
管の下部からｌｏＯｇ／１分間の速度で空気と共に送り
込み、浮遊状態で数秒間の熱処理を施した後加熱管の上
部から回収した。尚、加熱管による熱処理温度は１００
℃単位で９００℃から１８００℃とした。The produced dried gel was directly heated to an inner diameter of 10 c + + and a length of 2001 without performing heat treatment at a temperature of 800 ° C. The gel was placed in a vertical electric furnace with an inner diameter of 8 CIT and a length of 15 cm.
It was fed together with air from the bottom of the heating tube at a rate of loOg/1 minute into a heat-resistant heating tube made of 0 cm of alumina material, heat-treated for several seconds in a floating state, and then recovered from the top of the heating tube. The heat treatment temperature using the heating tube was 100
The temperature range was 900°C to 1800°C in degrees Celsius.
得られた各球状シリカガラスの空洞状態と、ガラス質に
ついて調べたところ、熱処理温度が１０００〜１５００
℃では得られた球状シリカガラスはガラス質であったが
発泡していた。また熱処理温度が１６００℃以上では得
られた球状シリカガラスは透明化されていたが、空洞状
態に形成されることなく中実状態であった。また熱処理
温度が９００℃以下では得られた球状シリカガラスは緻
密化されず、多孔質であった。When we investigated the hollow state and glass quality of each spherical silica glass obtained, we found that the heat treatment temperature was 1000 to 1500.
At ℃, the obtained spherical silica glass was glassy but foamed. Further, when the heat treatment temperature was 1600° C. or higher, the obtained spherical silica glass was transparent, but was solid without being formed in a hollow state. Further, when the heat treatment temperature was 900° C. or lower, the obtained spherical silica glass was not densified and was porous.
実施例および比較例から明らかなように、ゲル分散媒液
より分離されたゲルを湿度９０％、温度６０℃で乾燥し
た後、温度８００℃の熱処理と、更に温度１０００〜１
７００℃で浮遊状態での熱処理を施す本発明の実施例の
方法では中空球状シリカガラスが得られたのに対して、
ゲル分散媒液より分離し、乾燥されたゲルに直接高温度
の焼成を施す比較例の方法では発泡状態または中実状の
球状シリカガラスしか得られなかった。As is clear from the Examples and Comparative Examples, after drying the gel separated from the gel dispersion medium at a humidity of 90% and a temperature of 60°C, heat treatment at a temperature of 800°C and further heat treatment at a temperature of 1000 to 1
In contrast, hollow spherical silica glass was obtained by the method of the embodiment of the present invention in which heat treatment was carried out in a floating state at 700°C.
In the method of the comparative example in which the gel separated from the gel dispersion medium and dried is directly subjected to high-temperature firing, only foamed or solid spherical silica glass was obtained.
（発明の効果）
このように本発明の封止材用充填材は、中空球状シリカ
ガラスである。従って内部が空洞で、ガラスは透明で、
かつ強度が大きいので、半導体素子の封止材用充填材と
して用いたときは封止材用充填材自体の誘電率を小さく
出来るから半導体素子の誘電損失を低減させ、発熱性が
低減される等の効果を有する。(Effects of the Invention) As described above, the filler for sealing material of the present invention is hollow spherical silica glass. Therefore, the interior is hollow and the glass is transparent.
In addition, since it has high strength, when used as a filler for a semiconductor element encapsulant, the dielectric constant of the encapsulant filler itself can be reduced, which reduces the dielectric loss of the semiconductor element and reduces heat generation. It has the effect of
また、中空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で分散
させてゲルを生成させ、得られたゲルを分離し、該ゲル
を湿度５０％以上、温度４０〜９０℃の条件下で乾燥し
た後、焼成するようにしたので、従来法では得られなか
った中空球状シリカガラスを球体同士が凝集することな
く極めて簡単に製造することが出来る等の効果を有する
。In addition, the method for manufacturing hollow spherical silica glass involves dispersing a sol obtained by hydrolyzing a silicate ester raw material solution in a dispersion medium to generate a gel, separating the resulting gel, and dispersing the gel at a humidity of 50%. As mentioned above, since firing is performed after drying at a temperature of 40 to 90°C, hollow spherical silica glass, which could not be obtained by conventional methods, can be produced extremely easily without agglomeration of the spheres. It has the effect of
また、前記焼成を温度９００℃以下の熱処理と、次いで
温度１０００〜１７００℃で浮遊状態で熱処理とするこ
とによって、良好な中空球状シリカガラスが得られる。In addition, a good hollow spherical silica glass can be obtained by performing the above-mentioned firing as a heat treatment at a temperature of 900°C or less, and then a heat treatment in a floating state at a temperature of 1000 to 1700°C.
笛１図讐は中空球状シリカの空洞部分の大きさ状態を示
す図である。
特 許 出 願 人 日本無機株式会社ＯＨｍ
２０トｍFigure 1 is a diagram showing the size of the hollow part of the hollow spherical silica. Patent applicant Nippon Inuki Co., Ltd. OHm 20 tons
Claims (1)
を分散媒中で分散させてゲルを生成させ、得られたゲル
を分離し、湿度５０％以上、温度４０〜９０℃の条件下
で乾燥させた後、焼成することを特徴とする中空球状シ
リカガラスの製造方法。 ３、前記焼成は９００℃以下の温度で熱処理した後、次
いで温度１０００〜１７００℃で浮遊状態で熱処理する
ことにより行うことを特徴とする請求項２に記載の中空
球状シリカガラスの製造方法。[Claims] 1. A filler for a sealant made of hollow spherical silica glass. 2. The sol obtained by hydrolyzing the silicate ester raw material solution is dispersed in a dispersion medium to form a gel, and the resulting gel is separated and heated under conditions of a humidity of 50% or more and a temperature of 40 to 90°C. A method for producing hollow spherical silica glass, which comprises drying and then firing. 3. The method for producing hollow spherical silica glass according to claim 2, wherein the firing is performed by heat treatment at a temperature of 900°C or lower, and then heat treatment in a floating state at a temperature of 1000 to 1700°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4393989A JPH02225327A (en) | 1989-02-23 | 1989-02-23 | Production of filler for sealing material and hollow spherical silica glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4393989A JPH02225327A (en) | 1989-02-23 | 1989-02-23 | Production of filler for sealing material and hollow spherical silica glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02225327A true JPH02225327A (en) | 1990-09-07 |
| JPH0550447B2 JPH0550447B2 (en) | 1993-07-29 |
Family
ID=12677669
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4393989A Granted JPH02225327A (en) | 1989-02-23 | 1989-02-23 | Production of filler for sealing material and hollow spherical silica glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02225327A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001342010A (en) * | 2000-05-30 | 2001-12-11 | Kyocera Corp | Inorganic hollow powder and its production method |
-
1989
- 1989-02-23 JP JP4393989A patent/JPH02225327A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001342010A (en) * | 2000-05-30 | 2001-12-11 | Kyocera Corp | Inorganic hollow powder and its production method |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0550447B2 (en) | 1993-07-29 |
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