JP2968892B2 - Silica glass composite - Google Patents
Silica glass compositeInfo
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- JP2968892B2 JP2968892B2 JP26787692A JP26787692A JP2968892B2 JP 2968892 B2 JP2968892 B2 JP 2968892B2 JP 26787692 A JP26787692 A JP 26787692A JP 26787692 A JP26787692 A JP 26787692A JP 2968892 B2 JP2968892 B2 JP 2968892B2
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- silica glass
- composite
- purity
- synthetic
- ceramics
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Description
【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION
【０００１】[0001]
【産業上の利用分野】本発明は、耐熱性に優れたシリカ
ガラス複合体に関する。The present invention relates to a silica glass composite having excellent heat resistance.
【０００２】[0002]
【従来の技術】従来、石英ガラスは、高い純度を有し、
熱膨張率が極めて小さく耐急熱急冷性に優れ、かつ光特
に紫外線透過率が大きいところから、半導体工業用石英
ガラス、光学用透明石英ガラス、ランプ用石英ガラス、
熱処理治具用石英ガラス等多方面に使用されてきた。そ
してその原料としては透明石英ガラスでは天然の水晶等
が、また不透明石英ガラスではケイ石等が用いられてい
た。2. Description of the Related Art Conventionally, quartz glass has a high purity,
Since the coefficient of thermal expansion is extremely small, the resistance to rapid thermal quenching is excellent, and the transmittance of light, especially ultraviolet light, is large, quartz glass for semiconductor industry, transparent quartz glass for optics, quartz glass for lamps,
It has been used in various fields such as quartz glass for heat treatment jigs. As raw materials, natural quartz and the like have been used for transparent quartz glass, and quartzite and the like have been used for opaque quartz glass.
【０００３】近年、高純度のシリカを人工的に合成する
技術が確立し、四塩化ケイ素等を原料として高純度のシ
リカガラスが作られるようになった。しかしながら、こ
のシリカガラス（以下合成シリカガラスという）は、水
晶等の結晶質石英を溶融した溶融石英ガラス（以下溶融
石英ガラスという）に比べ、純度等の点で優れているも
のの、耐熱性に劣るという欠点を有していた。In recent years, a technique for artificially synthesizing high-purity silica has been established, and high-purity silica glass has been produced using silicon tetrachloride or the like as a raw material. However, this silica glass (hereinafter, referred to as synthetic silica glass) is superior in terms of purity and the like to fused silica glass obtained by melting crystalline quartz such as quartz (hereinafter, referred to as fused silica glass), but is inferior in heat resistance. Had the disadvantage that
【０００４】[0004]
【発明が解決しようとする課題】上記事情に鑑み、本発
明者等は、合成シリカガラスで溶融石英ガラス以上の耐
熱性を有するシリカガラスを提供すべく鋭意研究を重ね
たところ、合成シリカガラスに特定のセラミックスを複
合することにより前記欠点が解決できることを発見し
た。SUMMARY OF THE INVENTION In view of the above circumstances, the present inventors have conducted intensive studies to provide a synthetic silica glass having a heat resistance higher than that of fused silica glass. It has been found that the above disadvantages can be solved by combining specific ceramics.
【０００５】本発明の目的は、耐熱性に優れた新規なシ
リカガラス複合体を提供することにある。It is an object of the present invention to provide a novel silica glass composite having excellent heat resistance.
【０００６】[0006]
【課題を解決するための手段】上記目的を達成する本発
明は、シリカガラスマトリックスと非反応性の高純度セ
ラミックスとからなるシリカガラス複合体に係る。The present invention, which achieves the above object, relates to a silica glass composite comprising a silica glass matrix and a non-reactive high-purity ceramic.
【０００７】本発明の「セラミックス」とは、融点が約
２０００℃以上のセラミックスをいう。そして、このセ
ラミックスの形状は好ましくは長繊維、短繊維、ウイス
カーがよいが、粒子状でも同様な効果を得ることができ
る。The “ceramics” of the present invention refers to ceramics having a melting point of about 2000 ° C. or higher. The shape of the ceramic is preferably a long fiber, a short fiber, or a whisker.
【０００８】また「非反応性」とは、高温においてシリ
カガラスと化学反応をしない性質、特に反応ガスを生成
しない性質をいう。[0008] The term "non-reactive" refers to the property of not chemically reacting with silica glass at a high temperature, particularly the property of not producing a reactive gas.
【０００９】さらに、「高純度」とは、主成分の重量比
率が９７％以上のセラミックスのことをいう。ただし、
少なくともアルミナ（Ａｌ2Ｏ3）を８０ｗｔ．％以上含
有するアルミナ系セラミックス（例えば、Ａｌ2Ｏ3８０
ｗｔ．％，ＳｉＯ2２０ｗｔ．％）やジルコニア系セラ
ミックス（例えば、ＺｒＯ2９２ｗｔ．％，Ｙ2Ｏ3８ｗ
ｔ％）のように、約３ｗｔ．％以上の副成分は、本発明
の主成分に含めて扱うものとする。[0009] Further, "high purity" refers to ceramics whose main component has a weight ratio of 97% or more. However,
At least 80 wt.% Of alumina (Al 2 O 3 ). % Or more of alumina-based ceramics (for example, Al 2 O 3 80
wt. %, SiO 2 20 wt. %) And zirconia ceramics (e.g., ZrO 2 92wt.%, Y 2 O 3 8w
t%), about 3 wt. % Or more of the subcomponents shall be included in the main components of the present invention.
【００１０】他方、「低純度」とは、アルカリ金属元素
および遷移金属元素を３ｗｔ．％以上含有するセラミッ
クスをいう。[0010] On the other hand, "low purity" means that 3 wt. % Ceramics.
【００１１】前記非反応性の高純度セラミックスとして
は各種のセラミックスが挙げられるが、好ましくはマグ
ネシア系セラミックス、アルミナ系セラミックス、ジル
コニア系セラミックス等がよい。そしてこれら複合させ
るセラミックスは、高純度である必要がある。不純物が
存在すると、高温下で再結晶化が起こったり、あるいは
不純物が外部へ拡散することがある。前記不純物として
最も問題になる元素は、アルカリ金属のＬｉ，Ｎａ，
Ｋ，および遷移金属元素のＣｒ，Ｃｕ，Ｚｎ等である。
好ましいセラミックスであるファイバ−形状のセラミッ
クスと塊状透明合成シリカガラスの基本的な物性値を表
１に示す。As the non-reactive high-purity ceramics, various ceramics can be mentioned, but magnesia-based ceramics, alumina-based ceramics, zirconia-based ceramics and the like are preferable. These composite ceramics need to be of high purity. If an impurity is present, recrystallization may occur at a high temperature, or the impurity may diffuse outside. The most problematic elements as the impurities are the alkali metals Li, Na,
K and transition metal elements such as Cr, Cu, and Zn.
Table 1 shows basic physical properties of fiber-shaped ceramics and bulk transparent synthetic silica glass, which are preferable ceramics.
【００１２】[0012]
【表１】 ※ 上記表１のシリカガラスの融点は軟化点を表す。[Table 1] * The melting point of the silica glass in Table 1 above indicates the softening point.
【００１３】本発明のシリカガラス複合体は、高純度の
セラミックスを０．０１〜４０ｗｔ．％、好ましくは
０．１〜１０ｗｔ．％含有し、１１５０℃における粘度
が１０13.5ポアズ以上、１２８０℃における粘度が１０
11.5ポアズ以上である。そして、この合成シリカガラス
複合体のうち、その光透過率が厚さ１ｍｍ，波長５８８
ｎｍにおいて６０％以上であるシリカガラス複合体は、
特に透明メタルハライドランプ用放電管用ガラスとして
有用である。The silica glass composite of the present invention contains 0.01 to 40 wt. %, Preferably 0.1 to 10 wt. %, And a viscosity at 1150 ° C. of 10 13.5 poise or more and a viscosity at 1280 ° C. of 10
11.5 poise or more. The light transmittance of the synthetic silica glass composite is 1 mm in thickness and 588 in wavelength.
The silica glass composite which is 60% or more in nm is
Particularly, it is useful as a glass for a discharge tube of a transparent metal halide lamp.
【００１４】上記シリカガラス複合体において、高純度
セラミックの含有量が４０ｗｔ．％以上では、透明ガラ
ス化が困難となり、またシリカガラスとセラミックスの
熱膨張率差によりクラックの発生が起こり易くなる。高
純度セラミックの含有量が０．０１ｗｔ．％以下では粘
度の向上が見られない。In the above silica glass composite, the content of the high-purity ceramic is 40 wt. %, The vitrification becomes difficult, and cracks easily occur due to the difference in thermal expansion coefficient between silica glass and ceramics. The content of high-purity ceramic is 0.01 wt. %, No improvement in viscosity is observed.
【００１５】上記シリカガラス複合体において粘度が上
記範囲以下では高温使用時の熱変形が大きく、その使用
が制限される。When the viscosity of the above silica glass composite is lower than the above range, thermal deformation at the time of use at a high temperature is large, and its use is restricted.
【００１６】上記シリカガラス複合体が高純度の要求さ
れない分野に使用される場合には、必ずしもシリカマト
リックスを合成シリカガラスとする必要がなく、溶融石
英ガラスを使用しても良い。この場合、シリカガラス複
合体の耐熱性は一層向上する。When the silica glass composite is used in a field where high purity is not required, the silica matrix does not necessarily need to be synthetic silica glass, and fused silica glass may be used. In this case, the heat resistance of the silica glass composite is further improved.
【００１７】上述のとおり本発明のシリカガラス複合体
は、高い粘性を示すところから、半導体工業用ガラス、
熱処理用治具用ガラス等として有用であり、またその透
明性が優れているところからメタルハライドランプ放電
管用ガラス、水銀ランプ放電管用としても有用である。As described above, the silica glass composite of the present invention exhibits high viscosity,
It is useful as a glass for a heat treatment jig and the like, and is also useful as a glass for a metal halide lamp discharge tube and a mercury lamp discharge tube because of its excellent transparency.
【００１８】本発明のシリカガラス複合体は、例えば原
料のシリカガラスを粉砕し、その粒度を調整し、これに
予め長さ等を調整した非反応性の高純度セラミックスを
均一混合し、加熱溶融しガラス化する等の製造法により
製造することができる。The silica glass composite of the present invention is obtained, for example, by pulverizing raw material silica glass, adjusting its particle size, uniformly mixing non-reactive high-purity ceramics whose length and the like have been adjusted in advance, and then heating and melting. It can be manufactured by a manufacturing method such as vitrification.
【００１９】物性の測定 （１） 透過率測定 ： ＨＩＴＡＣＨＩ Ｍｏｄｅｌ
Ｕ−３２１０分光光度計により、厚さ１ｍｍの両面研
磨仕上げ試料に波長５８８ｎｍの光を透過して測定し
た。 （２） 粘度測定 ： ＡＳＴＭのＮｏ．Ｃ５９８に
準じビームベンデイング法により、１１５０℃と１２８
０℃における粘度を測定した。Measurement of physical properties (1) Measurement of transmittance: HITACHI Model
The measurement was performed using a U-3210 spectrophotometer by transmitting light having a wavelength of 588 nm to a 1 mm-thick double-side polished sample. (2) Viscosity measurement: ASTM No. According to the beam bending method according to C598, 1150 ° C and 128
The viscosity at 0 ° C. was measured.
【００２０】[0020]
【実施例１〜７】純度９９．９９９９ｗｔ．％の合成シ
リカガラスを粉砕機で粉砕し、粒度を＃６０〜１５０
（タイラ−メッシュ ０．２５ｍｍ〜０．１０５ｍｍ）
に調整した。Examples 1 to 7 Purity 99.9999 wt. % Of synthetic silica glass is crushed by a crusher to obtain a particle size of # 60 to 150.
(Tyler mesh 0.25mm to 0.105mm)
Was adjusted.
【００２１】一方、Ａｌ2Ｏ3９５ｗｔ．％，ＳｉＯ2５
ｗｔ．％の高純度の合成アルミナ繊維を直径１０μｍ，
長さ１００〜１０００μｍに調整した。これを前記調整
した合成シリカガラス粉末に、０ｗｔ．％，０．０１ｗ
ｔ．％，０．１ｗｔ．％，１ｗｔ．％，１０ｗｔ．％，
２０ｗｔ．％，５０ｗｔ．％加え、Ｖ型ミキサー機で混
合した後、加熱溶融しガラス化図った。得られたシリカ
ガラス複合体の物性値を表２に示す。[0021] On the other hand, Al 2 O 3 95wt. %, SiO 2 5
wt. % Synthetic alumina fiber of 10% in diameter,
The length was adjusted to 100 to 1000 μm. This was added to the prepared synthetic silica glass powder in an amount of 0 wt. %, 0.01w
t. %, 0.1 wt. %, 1 wt. %, 10 wt. %,
20 wt. %, 50 wt. %, Mixed by a V-type mixer, and then heated and melted for vitrification. Table 2 shows the physical property values of the obtained silica glass composite.
【００２２】[0022]
【参考例１】Ａｌ2Ｏ3９５ｗｔ．％であり，残りがＮａ
2Ｏ、Ｋ2Ｏ等のアルカリ金属化合物からなる低純度のア
ルミナ繊維と、実施例１の合成シリカガラスとを均一混
合し、加熱溶融しガラス化して複合体を得た。得られた
複合体の物性値を表２に示す。Reference Example 1 Al 2 O 3 95 wt. % And the remainder is Na
A low-purity alumina fiber composed of an alkali metal compound such as 2 O or K 2 O and the synthetic silica glass of Example 1 were uniformly mixed, heated and melted to obtain a composite. Table 2 shows the physical property values of the obtained composite.
【００２３】[0023]
【表２】 [Table 2]
【００２４】[0024]
【実施例８】純度９９ｗｔ．％以上の合成マグネシア繊
維を直径１〜１０μｍ，長さ１００〜１０００μｍに調
整し、これを実施例１の合成シリカガラス粉末に１ｗ
ｔ．％を混合し、加熱溶融してガラス化を図り、複合体
を得た。得られたシリカガラス複合体の物性値を表３に
示す。Example 8 Purity 99 wt. % Of synthetic magnesia fiber is adjusted to a diameter of 1 to 10 μm and a length of 100 to 1000 μm.
t. %, And the mixture was heated and melted for vitrification to obtain a composite. Table 3 shows the physical property values of the obtained silica glass composite.
【００２５】[0025]
【実施例９】合成アルミナ系繊維（組成Ａｌ2Ｏ3８０ｗ
ｔ．％，ＳｉＯ2２０ｗｔ．％）を実施例１の合成シリ
カガラスと混合し、実施例８と同様にシリカガラス復合
体をえた。得られた復合体の物性値を表３に示す。Embodiment 9 Synthetic alumina fiber (composition Al 2 O 3 80w)
t. %, SiO 2 20 wt. %) Was mixed with the synthetic silica glass of Example 1 to obtain a fused silica glass in the same manner as in Example 8. Table 3 shows the physical property values of the obtained composite.
【００２６】[0026]
【実施例１０】合成ジルコニア（ＺｒＯ2９２ｗｔ％，
Ｙ2Ｏ3８ｗｔ％）繊維を直径１〜１０μｍ，長さ１００
〜１０００μｍに調整し、実施例９と同様にシリカガラ
ス複合体を得た。得られた複合体の物性値を表３に示
す。Embodiment 10 Synthetic zirconia (ZrO 2 92 wt%,
Y 2 O 3 8wt%) Fiber diameter 1 to 10 [mu] m, length 100
The thickness was adjusted to 1000 μm, and a silica glass composite was obtained in the same manner as in Example 9. Table 3 shows the physical property values of the obtained composite.
【００２７】[0027]
【参考例２】純度９９ｗｔ．％以上の合成炭化ケイ素繊
維を直径１〜１０μｍ，長さ５〜２００μｍに調整し、
実施例１の合成シリカガラスと混合し、加熱溶融してガ
ラス化を図った。しかしながら、この合成炭化ケイ素繊
維は合成シリカガラスと反応するため得られた複合体は
多孔体となった。その結果を表３に示す。Reference Example 2 Purity 99 wt. % Of synthetic silicon carbide fiber is adjusted to a diameter of 1 to 10 μm and a length of 5 to 200 μm,
It was mixed with the synthetic silica glass of Example 1 and melted by heating to achieve vitrification. However, since the synthetic silicon carbide fiber reacted with the synthetic silica glass, the obtained composite became porous. Table 3 shows the results.
【００２８】[0028]
【参考例３】純度９９ｗｔ．％以上の合成チッ化ケイ素
繊維を直径０．１〜１μｍｍ，長さ５〜２００μｍに調
整し、実施例１の合成シリカガラスと混合し、加熱溶融
しガラス化を図った。しかしながら、この合成チッ化ケ
イ素繊維は合成シリカガラスと反応するため得られた複
合体は多孔体となった。その結果を表３に示す。Reference Example 3 Purity 99 wt. % Of synthetic silicon nitride fiber was adjusted to a diameter of 0.1 to 1 μm and a length of 5 to 200 μm, mixed with the synthetic silica glass of Example 1, and heated and melted for vitrification. However, since the synthetic silicon nitride fiber reacted with the synthetic silica glass, the obtained composite became porous. Table 3 shows the results.
【００２９】[0029]
【表３】 注） 参考例４のシリカガラスは市販の超高純度合成シ
リカガラスであり、また参考例５のシリカガラスは半導
体工業用石英ガラスとして市販されているガラスであ
る。[Table 3] Note) The silica glass of Reference Example 4 is a commercially available ultra-high purity synthetic silica glass, and the silica glass of Reference Example 5 is a glass commercially available as quartz glass for the semiconductor industry.
【００３０】[0030]
【実施例１１〜１４】実施例１の合成シリカガラス粉体
に純度９９．９９ｗｔ．％のアルミナ粉体（粒径０．５
〜５μｍ）を各０ｗｔ．％、０．１ｗｔ．％、１ｗｔ．
％、および１０ｗｔ．％を加え、Ｖ型ミキサーで均一に
混合した。これらの混合体を真空炉内に設置し約１８０
０℃の温度にて溶融透明ガラス化し、シリカガラス複合
体を得た。Examples 11 to 14 The synthetic silica glass powder of Example 1 had a purity of 99.99 wt. % Alumina powder (particle size 0.5
0 to 5 μm). %, 0.1 wt. %, 1 wt.
%, And 10 wt. % And uniformly mixed with a V-type mixer. These mixtures are placed in a vacuum furnace and are
The mixture was melted and vitrified at a temperature of 0 ° C. to obtain a silica glass composite.
【００３１】得られたシリカガラス複合体の外観検査、
光透過率、および１１５０℃における粘度測定を行っ
た。その結果を表４に示す。Inspection of the appearance of the obtained silica glass composite,
The light transmittance and the viscosity at 1150 ° C. were measured. Table 4 shows the results.
【００３２】[0032]
【実施例１５】純度９９．９９ｗｔ．％のマグネシア粉
体（粒径０．５〜５μｍ）を実施例１の合成シリカガラ
スとＶ型ミキサーで均一混合し、この混合物を加熱溶融
し、透明ガラス化した。Example 15 Purity 99.99 wt. % Of magnesia powder (particle size: 0.5 to 5 μm) was uniformly mixed with the synthetic silica glass of Example 1 using a V-type mixer, and the mixture was heated and melted to form a transparent glass.
【００３３】得られたシリカガラス複合体の外観検査、
光透過率、および１１５０℃における粘度測定を行っ
た。その結果を表４に示す。Inspection of the appearance of the obtained silica glass composite,
The light transmittance and the viscosity at 1150 ° C. were measured. Table 4 shows the results.
【００３４】[0034]
【実施例１６】純度９９．９９ｗｔ．％のジルコニア粉
体（ＺｒＯ2９２ｗｔ％，Ｙ2Ｏ3８ｗｔ％），粒径０．
５〜５μｍを実施例１の合成シリカガラスとＶ型ミキサ
ーで均一混合し、この混合物を加熱溶融し、透明ガラス
化した。Example 16 Purity 99.99 wt. % Of zirconia powder (92 wt% of ZrO 2 , 8 wt% of Y 2 O 3 ), particle size of 0.
5 to 5 μm was uniformly mixed with the synthetic silica glass of Example 1 using a V-type mixer, and this mixture was heated and melted to form a transparent glass.
【００３５】得られたシリカガラス複合体の外観検査、
光透過率、および１１５０℃における粘度測定を行っ
た。その結果を表４に示す。Appearance inspection of the obtained silica glass composite,
The light transmittance and the viscosity at 1150 ° C. were measured. Table 4 shows the results.
【００３６】[0036]
【表４】 [Table 4]
【００３７】[0037]
【発明の効果】本発明は、上記実施例から明らかなよう
に非反応性の高純度セラミックスを０．０１〜４０ｗ
ｔ．％合成シリカガラスに配合した複合体は透明性が高
いとともに粘度も著しく向上していることがわかる。特
に、セラミックスファイバ−を０．１〜１０ｗｔ．％混
入した合成シリカガラス複合体は、高い透明性を有し、
かつ溶融石英ガラス以上の優れた耐熱性を示す。According to the present invention, as is apparent from the above examples, the non-reactive high-purity ceramics are used in an amount of 0.01 to 40 watts.
t. It can be seen that the composite blended with the% synthetic silica glass has high transparency and significantly improved viscosity. In particular, the ceramic fiber is 0.1 to 10 wt. % Synthetic silica glass composite has high transparency,
In addition, it shows excellent heat resistance more than fused silica glass.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) C03C 14/00 ──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. 6 , DB name) C03C 14/00
Claims (3)
で、融点が約２０００℃以上のセラミックスが、シリカ
ガラスマトリックスに対して０．０１〜４０ｗｔ％存在
し、１１５０℃における粘度が１０ 13.5 ポアズ以上、１
２８０℃における粘度が１０ 11.8 ポアズ以上であること
を特徴とするシリカガラス複合体。1. A non-reactive ceramic having a melting point of about 2,000 ° C. or more in a silica glass matrix is present in an amount of 0.01 to 40% by weight based on the silica glass matrix.
And a viscosity at 1150 ° C. of 10 13.5 poise or more,
A silica glass composite having a viscosity at 280 ° C. of 10 11.8 poise or more .
ス、アルミナ系セラミックス又はジルコニア系セラミッ
クスのいずれかであることを特徴とする請求項１記載の
シリカガラス複合体。2. The silica glass composite according to claim 1, wherein the ceramic is one of magnesia-based ceramics, alumina-based ceramics, and zirconia-based ceramics.
て、透過率が厚さ１ｍｍ、波長５８８ｎｍにおいて６０
％以上であることを特徴とする放電管用複合体。 3. The silica glass composite according to claim 1,
Has a transmittance of 60 at a thickness of 1 mm and a wavelength of 588 nm.
% Or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26787692A JP2968892B2 (en) | 1992-04-10 | 1992-09-11 | Silica glass composite |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4-116787 | 1992-04-10 | ||
| JP11678792 | 1992-04-10 | ||
| JP26787692A JP2968892B2 (en) | 1992-04-10 | 1992-09-11 | Silica glass composite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05339030A JPH05339030A (en) | 1993-12-21 |
| JP2968892B2 true JP2968892B2 (en) | 1999-11-02 |
Family
ID=26455037
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26787692A Expired - Fee Related JP2968892B2 (en) | 1992-04-10 | 1992-09-11 | Silica glass composite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2968892B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5900381A (en) * | 1997-08-26 | 1999-05-04 | General Electric Company | Opaque silica composition |
-
1992
- 1992-09-11 JP JP26787692A patent/JP2968892B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05339030A (en) | 1993-12-21 |
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