【０００１】[0001]
【産業上の利用分野】本発明はＬｉ2 Ｏ−Ａｌ2 Ｏ3 −
ＳｉＯ2 系結晶化ガラスに関するものである。The present invention relates to Li2 O—Al2 O3 −
It relates to an SiO2 -based crystallized glass.
【０００２】[0002]
【従来の技術】従来より、石油、薪、その他のストーブ
の前面窓、カラーフィルターやイメージセンサ用基板等
のハイテク製品用基板、電子部品焼成用セッター、電子
レンジ用棚板、電磁調理器用トッププレート、防火戸用
窓ガラス等の材料として、Ｌｉ2 Ｏ−Ａｌ2 Ｏ3 −Ｓｉ
Ｏ2 系の低膨張な結晶化ガラスが用いられている。例え
ば特公昭３９−２１０４９号公報、特公昭４０−２０１
８２号公報、特開平１−３０８８４５号公報等には、主
結晶としてβ−石英固溶体（Ｌｉ2 Ｏ・Ａｌ2 Ｏ3 ・ｎ
ＳｉＯ2 ［ただしｎ≧２］）やβ−スポジュメン固溶体
（Ｌｉ2 Ｏ・Ａｌ2 Ｏ3 ・ｎＳｉＯ2 ［ただしｎ≧
４］）を析出してなるＬｉ2 Ｏ−Ａｌ2 Ｏ3 −ＳｉＯ2
系結晶化ガラスが開示されている。2. Description of the Related Art Conventionally, petroleum, firewood, other windows of stoves, substrates for high-tech products such as color filters and image sensor substrates, setters for firing electronic components, shelf plates for microwave ovens, top plates for electromagnetic cookers. Li2 O—Al2 O3 —Si as a material for window glass for fire doors, etc.
O2 -based low expansion crystallized glass is used. For example, Japanese Patent Publication No. 39-21049, Japanese Patent Publication No. 40-201
No. 82, Japanese Patent Application Laid-Open No. 1-308845, and the like disclose a β-quartz solid solution (Li2 O.Al2 O3 .n) as a main crystal.
SiO2 [where n ≧ 2] or β-spodumene solid solution (Li2 O · Al2 O3 · nSiO2 [where n ≧ 2]
4]) deposited Li2 O—Al2 O3 —SiO2
A system-crystallized glass is disclosed.
【０００３】[0003]
【発明が解決しようとする課題】上記したＬｉ2 Ｏ−Ａ
ｌ2 Ｏ3 −ＳｉＯ2 系結晶化ガラスは、熱膨張係数が低
く、機械的強度も高いために優れた熱的特性を有してい
る。また結晶化工程における熱処理条件を変更すること
によって析出結晶を変化させることができるため、同一
組成の原ガラスから、透明な結晶化ガラスと白色不透明
な結晶化ガラスの両方を製造することが可能であり、そ
れぞれの用途に応じて使い分けることができるものであ
る。The above-mentioned Li2 O-A
l2 O3 -SiO2 based crystallized glass has low coefficient of thermal expansion, and has excellent thermal properties for high mechanical strength. In addition, since the precipitated crystals can be changed by changing the heat treatment conditions in the crystallization step, it is possible to produce both transparent crystallized glass and white opaque crystallized glass from raw glass having the same composition. They can be used for different purposes.
【０００４】ところで近年、エレクトロニクスや精密部
品の分野に透明な結晶化ガラスの需要が拡大しつつある
が、これに伴ってガラスの外観品位に対する要求が厳し
くなってきている。しかしながらこの系の結晶化ガラス
は一般に溶解性が悪く、ガラス中に泡欠陥が生じ易いと
いう問題がある。[0004] In recent years, the demand for transparent crystallized glass has been expanding in the field of electronics and precision parts, and accordingly, the demand for the appearance quality of glass has become strict. However, crystallized glass of this type generally has poor solubility, and has a problem that bubble defects are easily generated in the glass.
【０００５】本発明の目的は、泡欠陥がなく、外観品位
に優れたＬｉ2 Ｏ−Ａｌ2 Ｏ3 −ＳｉＯ2 系結晶化ガラ
スを提供することである。An object of the present invention is to provide a Li2 O—Al2 O3 —SiO2 crystallized glass having no bubble defects and excellent appearance quality.
【０００６】[0006]
【課題を解決するための手段】本発明者等は種々の実験
を行った結果、特定量のＭｇＯ、ＺｎＯ及びＢａＯを必
須成分として含有し、しかも、これら成分の合量を１．
６〜３．４重量％にすることにより、上記目的が達成で
きることを見いだし、本発明として提案するものであ
る。As a result of various experiments, the present inventors have found that a specific amount of MgO, ZnO and BaO is containedas an essential component, and the total amount of these components is 1.
It has been found that the above object can be achieved byadjusting the content to 6 to3.4% by weight , and the present invention is proposed.
【０００７】即ち、本発明のＬｉ2Ｏ−Ａｌ2Ｏ3−Ｓｉ
Ｏ2系結晶化ガラスは、重量百分率で、ＳｉＯ2 ６０〜
７０％、Ａｌ2Ｏ3 １７〜２７％、Ｌｉ2Ｏ ３〜６
％、ＭｇＯ ０．１〜０．９％、ＺｎＯ １〜２％、Ｂ
ａＯ ０．１〜０．９％、ＭｇＯ＋ＺｎＯ＋ＢａＯ
１．６〜３．４％、ＴｉＯ2 １．３〜２．９％、Ｚｒ
Ｏ2１〜３％、Ｐ2Ｏ5 ０．０５〜１．９％、Ｎａ2Ｏ
０．０５〜１％、Ｋ2Ｏ ０．１〜１％の組成を含有
し、主結晶としてβ−石英固溶体又はβ−スポジュメン
固溶体を析出してなることを特徴とする。That is, the Li2 O—Al2 O3 —Si of the present invention
O2 -based crystallized glass has a SiO2 content of 60 to 60% by weight.
70%, Al 2 O 3 17~27 %, Li 2 O 3~6
%, MgO 0.1-0.9%, ZnO 1-2%, B
aO 0.1-0.9%,MgO + ZnO + BaO
1.6~3.4%, TiO 2 1.3~2.9%, Zr
O 2 1~3%, P 2 O 5 0.05~1.9%, Na 2 O
0.05 to 1%,containing a composition of K2 O 0.1 to 1%
And a β-quartz solid solution or β-spodumene solid solution asa main crystal.
【０００８】[0008]
【作用】本発明において、組成範囲を上記のように限定
した理由を以下に述べる。The reason for limiting the composition range as described above in the present invention will be described below.
【０００９】ＳｉＯ2 はガラスのネットワークフォーマ
ーであるとともに結晶を構成する成分であるが、その含
有量が６０％より少ないと熱膨張係数が高くなるととも
に機械的強度が低くなり、７０％より多いとガラスの溶
解が困難となって泡や失透物等の欠陥が発生する。[0009] SiO2 is a glass network former and a component constituting a crystal. If its content is less than 60%, the thermal expansion coefficient increases, the mechanical strength decreases, and the content exceeds 70%. Then, it becomes difficult to melt the glass, and defects such as bubbles and devitrified materials are generated.
【００１０】Ａｌ2 Ｏ3 は結晶を構成する成分である
が、１７％より少ないとガラスの失透性が強くなるとと
もに化学耐久性が低下し、２７％より多いとガラスの粘
性が高くなりすぎて均一なガラスが得られなくなる。[0010] Al2 O3 is a component constituting the crystal. If the content is less than 17%, the devitrification of the glass is increased and the chemical durability is reduced. If the content is more than 27%, the viscosity of the glass is too high. And uniform glass cannot be obtained.
【００１１】Ｌｉ2 Ｏは結晶を構成する成分であるが、
３％より少ないと所望の結晶が析出し難くなるとともに
溶解性が悪くなる。一方、６％より多いとガラスの失透
性が強くなり、成型が困難になる。Li2 O is a component constituting a crystal.
If it is less than 3%, the desired crystals will not be easily precipitated and the solubility will be poor. On the other hand, if it is more than 6%, the devitrification of the glass becomes strong and molding becomes difficult.
【００１２】ＭｇＯは溶解性を向上させ、泡欠陥の発生
を防止する成分であるが、０．１％より少ないとその効
果がなく、泡が発生し易くなる。一方、ＭｇＯが０．９
％より多いと熱膨張係数が大きくなって熱的特性が低下
する。また透明結晶化ガラスの場合、ＴｉＯ2 の存在に
よってガラスが僅かに着色することがあるが、ＭｇＯの
含有量が上記範囲を超えるとこの着色が濃くなって透明
性が損なわれる。MgO is a component that improves the solubility and prevents the occurrence of bubble defects. If the content is less than 0.1%, the effect is not obtained, and bubbles are easily generated. On the other hand, when MgO is 0.9
%, The thermal expansion coefficient increases and the thermal characteristics deteriorate. In the case of transparent crystallized glass, the glass may be slightly colored due to the presence of TiO2. However, if the content of MgO exceeds the above range, the coloring becomes deeper and the transparency is impaired.
【００１３】ＺｎＯも溶解性を向上させ、泡欠陥の発生
を防止する成分であるが、１％より少ないとその効果が
なく、２％より多い場合は誘電損失が大きくなって電子
レンジ用途に使用するとホットスポットが発生してしま
う。また透明結晶化ガラスの場合、ＭｇＯと同様に着色
が濃くなり過ぎる。[0013] ZnO is also a component that improves the solubility and prevents the generation of bubble defects. However, less than 1% has no effect. Then, a hot spot is generated. In the case of a transparent crystallized glass, the coloring becomes too deep as in the case of MgO.
【００１４】ＢａＯも溶解性を向上させ、泡欠陥の発生
を防止する成分であるが、０．１％より少ないとその効
果がなく、０．９％より多いと熱膨張係数が高くなり過
ぎるとともに誘電損失が大きくなる。BaO is also a component that improves the solubility and prevents the occurrence of bubble defects. However, if it is less than 0.1%, it has no effect, and if it is more than 0.9%, the thermal expansion coefficient becomes too high, and The dielectric loss increases.
【００１５】なお、ＭｇＯとＺｎＯとＢａＯの合量は
１．６〜３．４％の範囲にする必要がある。その理由は
これらの合量が１．６％より少ないとガラスの溶解性が
悪くなり易く、３．４％より多いと結晶化の際に異種結
晶が析出し、強度や耐熱性が低下し易いためである。The total amount of MgO, ZnO and BaOneeds to be in the range of 1.6 to 3.4%. The reason is that if the total amount is less than 1.6%, the solubility of the glass tends to deteriorate, and if it exceeds 3.4%, heterogeneous crystals are precipitated during crystallization, and the strength and heat resistance tend to decrease. That's why.
【００１６】ＴｉＯ2 は核形成剤として作用するが、
１．３％より少ないと結晶化を促進する効果が得られ
ず、所望の結晶が得られなくなり、２．９％より多いと
液相温度が高くなり、成型作業が困難になる。また透明
結晶化ガラスの場合、ガラスが濃褐色に着色して透明性
が損なわれる。TiO2 acts as a nucleating agent,
If it is less than 1.3%, the effect of accelerating crystallization cannot be obtained, and desired crystals cannot be obtained. If it is more than 2.9%, the liquidus temperature becomes high, and the molding operation becomes difficult. In the case of transparent crystallized glass, the glass is colored dark brown, and the transparency is impaired.
【００１７】ＺｒＯ2 は核形成剤として作用するが、１
％より少ないと結晶化が安定して起こらない。また結晶
が粗大になる結果、透明な結晶化ガラスが得られなくな
る。一方、３％より多いとジルコニアの未溶解物が生
じ、ガラス中に失透物が発生する。ZrO2 acts as a nucleating agent,
%, Crystallization does not occur stably. Further, as a result of the coarse crystals, a transparent crystallized glass cannot be obtained. On the other hand, if it is more than 3%, undissolved zirconia is generated, and devitrified substances are generated in the glass.
【００１８】なおＴｉＯ2 とＺｒＯ2 の合量は、２．６
〜５％の範囲にあることが望ましい。これらの合量が
２．６％より少ないと十分な結晶化促進効果が得られ
ず、結晶量が少なくなって機械的強度が低下し易くな
る。一方、これら成分の合量が５％より多いと失透性が
強まり、均一な結晶化ガラスが得難くなる。The total amount of TiO2 and ZrO2 is 2.6
It is desirable to be in the range of 5%. If the combined amount is less than 2.6%, a sufficient crystallization promoting effect cannot be obtained, and the amount of crystals is reduced, so that the mechanical strength tends to decrease. On the other hand, if the total amount of these components is more than 5%, the devitrification will increase, and it will be difficult to obtain a uniform crystallized glass.
【００１９】Ｐ2 Ｏ5 は、核形成剤として含有されるＺ
ｒＯ2 の難溶解性を改善する効果があるが、０．０５％
より少ないとその効果がなく、１．９％より多いと分相
し易くなって均一なガラスが得られない。また結晶量が
多くなって透明な結晶化が得難くなる。なおＰ2 Ｏ5 の
含有量は、０．０５〜０．９％であることが望ましい。P2 O5 contains Z as a nucleating agent.
Effective for improving the poor solubility of rO2 , but 0.05%
If the amount is less than the above value, the effect is not obtained. If the amount is more than 1.9%, the phases are easily separated, so that a uniform glass cannot be obtained. Further, the amount of crystals increases, and it becomes difficult to obtain transparent crystallization. Note that the content of P2 O5 is desirably 0.05 to 0.9%.
【００２０】Ｎａ2 Ｏはガラスの溶解性を向上させる効
果があるが、０．０５％より少ないとその効果がなく、
１％より多いとガラスの熱膨張係数及び誘電損失が大き
くなる。Na2 O has the effect of improving the solubility of glass, but less than 0.05% has no effect.
If it exceeds 1%, the thermal expansion coefficient and the dielectric loss of the glass increase.
【００２１】Ｋ2 Ｏはガラスの溶解性を向上させる効果
があるが、０．１％より少ないとその効果がなく、１％
を超えると熱膨張係数及び誘電損失が大きくなる。K2 O has the effect of improving the solubility of glass, but if it is less than 0.1%, the effect is not obtained and 1%
If it exceeds, the coefficient of thermal expansion and the dielectric loss increase.
【００２２】なお、Ｎａ2 ＯとＫ2 Ｏの合量は０．５〜
２％であることが好ましい。これら成分の合量が０．５
％未満の場合はガラスの溶解性が悪化し易くなり、２％
を超えると結晶化ガラスの強度や耐熱性が低下し易くな
る。The total amount of Na2 O and K2 O is 0.5 to
Preferably it is 2%. When the total amount of these components is 0.5
If it is less than 2%, the melting property of the glass is liable to deteriorate, and 2%
If it exceeds 300, the strength and heat resistance of the crystallized glass tend to decrease.
【００２３】更に、本発明のＬｉ2 Ｏ−Ａｌ2 Ｏ3 −Ｓ
ｉＯ2 系結晶化ガラスは、上記成分以外にもＣａＯ、Ｐ
ｂＯ、Ｆ2 、Ｃｌ2 、ＣｅＯ2 等の任意成分を各々３％
以下含有させることが可能である。また清澄剤としてＡ
ｓ2 Ｏ3 やＳｂ2 Ｏ3 を合量で２％以下含有させること
によってガラスの溶解性、作業性、均一性を向上させる
ことができる。Furthermore, the Li2 O—Al2 O3 —S of the present invention
iO2 -based crystallized glass is not only CaO, P
Optional components such as bO, F2 , Cl2 and CeO2 are each 3%
The following can be contained. A as a fining agent
By including s2 O3 or Sb2 O3 in a total amount of 2% or less, the solubility, workability and uniformity of the glass can be improved.
【００２４】[0024]
【実施例】以下、本発明のＬｉ2 Ｏ−Ａｌ2 Ｏ3 −Ｓｉ
Ｏ2 系結晶化ガラスを実施例に基づいて説明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The Li2 O--Al2 O3 --Si of the present invention will now be described.
The O2 -based crystallized glass will be described based on examples.
【００２５】表１〜４は、本発明の実施例（試料Ｎｏ．
１〜６）及び比較例（試料Ｎｏ．７）を示している。Tables 1 to 4 show examples (sample Nos.) Of the present invention.
1 to 6) and a comparative example (sample No. 7).
【００２６】[0026]
【表１】[Table 1]
【００２７】[0027]
【表２】[Table 2]
【００２８】[0028]
【表３】[Table 3]
【００２９】[0029]
【表４】[Table 4]
【００３０】表中の各試料は次のようにして調製した。Each sample in the table was prepared as follows.
【００３１】表の組成になるようにガラス原料を調合
し、均一に混合した後、白金坩堝を用いて１５８０℃で
１６時間溶解した。次いで溶融したガラスをカーボン定
盤の上に流し出し、ステンレスローラーを用いて５ｍｍ
厚の板ガラスを得、徐冷炉で室温まで冷却した。続いて
各板ガラスを表に示す２通りの熱処理条件で結晶化させ
た後、炉冷して試料を得た。Glass raw materials were prepared so as to have the composition shown in the table, mixed uniformly, and then melted at 1580 ° C. for 16 hours using a platinum crucible. Next, the molten glass was poured on a carbon platen, and 5 mm using a stainless steel roller.
A thick plate glass was obtained and cooled to room temperature in a lehr. Subsequently, each plate glass was crystallized under the two heat treatment conditions shown in the table, and then cooled in a furnace to obtain a sample.
【００３２】次に各試料について、泡の発生個数、熱膨
張係数及び主結晶を求めた。Next, the number of bubbles generated, the coefficient of thermal expansion, and the main crystal of each sample were determined.
【００３３】なお泡の発生個数は、結晶化熱処理前の板
ガラスを用い、実体顕微鏡にて観察し、計数した。熱膨
張係数は、３０〜７５０℃における値を熱膨張計を用い
て求めた。主結晶は、Ｘ線回折法により同定した。The number of generated bubbles was counted by observing the glass sheet before the crystallization heat treatment with a stereoscopic microscope. The coefficient of thermal expansion was determined at 30 to 750 ° C. using a thermal dilatometer. The main crystal was identified by the X-ray diffraction method.
【００３４】表から明らかなように、各試料とも熱処理
条件を変えることによって、−５〜２×１０-7／℃の熱
膨張係数を有しβ−石英固溶体を主結晶とする透明結晶
化ガラスと、１１〜１３×１０-7／℃の熱膨張係数を有
しβ−スポジュメン固溶体を主結晶とする白色不透明な
結晶化ガラスの両方が得られた。As is clear from the table, the transparent crystallized glass having a thermal expansion coefficient of -5 to 2 × 10−7 / ° C. and a β-quartz solid solution as a main crystal was obtained by changing the heat treatment conditions for each sample. And a white opaque crystallized glass having a thermal expansion coefficient of 11 to 13 × 10−7 / ° C. and having a β-spodumene solid solution as a main crystal were obtained.
【００３５】しかし本発明の実施例である試料Ｎｏ．１
〜６は泡が殆ど認められなかったのに対し、比較例であ
る試料Ｎｏ．７は、泡が約３５０個／ｋｇもあった。However, in the case of the sample No. 1
Sample Nos. 6 to 6 were almost no bubbles, whereas Sample Nos. 7 had about 350 bubbles / kg.
【００３６】これらの事実は、本発明のＬｉ2Ｏ−Ａｌ2
Ｏ3−ＳｉＯ2系結晶化ガラスが、少量のＢａＯとＺｎＯ
とＭｇＯを必須成分として含有し、しかも、これら成分
の合量が１．６〜３．４％の範囲であるために、泡が大
幅に低減されることを示している。These facts indicate that the Li2 O—Al2 of the present invention is used.
O3 -SiO2 based crystallized glass, a small amount of BaO and ZnO
And MgO as essentialcomponents.
Indicate that the amount of foam is greatly reduced because thetotal amount of the polystyrene is in the range of 1.6 to 3.4% .
【００３７】[0037]
【発明の効果】以上説明したように、本発明のＬｉ2 Ｏ
−Ａｌ2 Ｏ3 −ＳｉＯ2 系結晶化ガラスは溶解性が良好
であり、泡欠陥が生じ難いため、外観品位に優れてい
る。それゆえストーブ前面窓やハイテク製品用基板とし
て好適である。As described above, the Li2 O of the present invention is used.
—Al2 O3 —SiO2 -based crystallized glass has good solubility and is unlikely to cause bubble defects, and thus has excellent appearance quality. Therefore, it is suitable as a stove front window or a substrate for high-tech products.
【００３８】さらに従来のＬｉ2 Ｏ−Ａｌ2 Ｏ3 −Ｓｉ
Ｏ2 系結晶化ガラスと同様に熱膨張係数が非常に低いた
め、電子部品焼成用セッター、電子レンジ用棚板、電磁
調理器用トッププレート等多くの工業用材料として使用
することも可能である。Further, conventional Li2 O—Al2 O3 —Si
Since it has a very low coefficient of thermal expansion similarly to O2 -based crystallized glass, it can be used as many industrial materials such as electronic component firing setters, microwave oven shelves, and electromagnetic cooker top plates.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平７−172862（ＪＰ，Ａ) 特開 昭49−99521（ＪＰ，Ａ) 特開 平４−214046（ＪＰ，Ａ) 特開 平２−293345（ＪＰ，Ａ) 特開 平６−329439（ＪＰ，Ａ) 特開 平４−285029（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C03C 1/00 - 14/00──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-7-172862 (JP, A) JP-A-49-99521 (JP, A) JP-A-4-214046 (JP, A) JP-A-2- 293345 (JP, A) JP-A-6-329439 (JP, A) JP-A-4-285029 (JP, A) (58) Fields investigated (Int. Cl.7 , DB name) C03C 1/00-14 / 00
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35293395AJP3269529B2 (en) | 1995-12-29 | 1995-12-29 | Li2O-Al2O3-SiO2-based crystallized glass |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35293395AJP3269529B2 (en) | 1995-12-29 | 1995-12-29 | Li2O-Al2O3-SiO2-based crystallized glass |
| Publication Number | Publication Date |
|---|---|
| JPH09188538A JPH09188538A (en) | 1997-07-22 |
| JP3269529B2true JP3269529B2 (en) | 2002-03-25 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35293395AExpired - Fee RelatedJP3269529B2 (en) | 1995-12-29 | 1995-12-29 | Li2O-Al2O3-SiO2-based crystallized glass |
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| JP (1) | JP3269529B2 (en) |
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