JP2007099557A - Tempered glass article and method for producing the same - Google Patents

Tempered glass article and method for producing the same Download PDF

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JP2007099557A
JP2007099557A JP2005290714A JP2005290714A JP2007099557A JP 2007099557 A JP2007099557 A JP 2007099557A JP 2005290714 A JP2005290714 A JP 2005290714A JP 2005290714 A JP2005290714 A JP 2005290714A JP 2007099557 A JP2007099557 A JP 2007099557A
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tempered glass
glass
glass article
producing
strain point
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Shinkichi Miwa
晋吉 三和
Masahiro Kobayashi
正宏 小林
Koichi Hashimoto
幸市 橋本
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Nippon Electric Glass Co Ltd
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Nippon Electric Glass Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass

Abstract

<P>PROBLEM TO BE SOLVED: To provide a tempered glass article which is hard to be broken because of its provision of a compression stress layer with sufficient dimensions by tempering, and in which the tempered effect is not damaged even if being subjected to treatment such as filming, and to provide a method for producing the same. <P>SOLUTION: The tempered glass article has a strain point of ≥550°C, and has a compressive stress layer of ≥100 MPa from the surface to a depth of 1 to 100 μm. Regarding the method for producing the tempered glass article, a plate glass having a composition of, by mass%, SiO<SB>2</SB>+Al<SB>2</SB>O<SB>3</SB>+ZrO<SB>2</SB>; 60 to 80%, MgO+CaO+SrO+BaO; 10 to 30%, and Li<SB>2</SB>O+Na<SB>2</SB>O; 0.5 to 15% is dipped in a melt of 400 to 550°C comprising potassium nitrate for 1 to 48 hr. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、強化ガラス物品およびその製造方法に関し、特に携帯機器のディスプレイ等の保護板に使用される強化ガラス物品およびその製造方法に関するものである。   The present invention relates to a tempered glass article and a method for producing the same, and more particularly to a tempered glass article used for a protective plate such as a display of a portable device and a method for producing the same.

近年、ディスプレイの主流であったブラウン管（ＣＲＴ）に代わって薄型ディスプレイが様々な用途に使用されている。具体的には液晶ディスプレイ（Ｌｉｑｕｉｄ Ｃｒｙｓｔａｌ Ｄｉｓｐｌａｙ、ＬＣＤ）や有機ＥＬディスプレイ（Ｏｒｇａｎｉｃ Ｌｉｇｈｔ Ｅｍｉｔｔｉｎｇ Ｄｉｏｄｅ、ＯＬＥＤ）などが挙げられる。これらのディスプレイにはいずれも肉厚の薄いガラス基板が使用される。   In recent years, thin displays have been used in various applications in place of cathode ray tubes (CRT), which have been the mainstream of displays. Specifically, a liquid crystal display (Liquid Crystal Display, LCD), an organic EL display (Organic Light Emitting Diode, OLED), etc. are mentioned. Each of these displays uses a thin glass substrate.

特に、携帯電話や携帯情報端末などの携帯機器に用いられるディスプレイには、機器本体の薄型化、軽量化の要求により、板厚０．７ｍｍ以下のガラス基板が用いられている。携帯機器が落下したり、圧迫されたりすることによって衝撃や外力が加わると、薄いガラス基板を用いたディスプレイの場合、ディスプレイ自体が破損したり、変形などによって画像が乱れたりするという問題を有していた。   In particular, a glass substrate having a thickness of 0.7 mm or less is used for a display used in a portable device such as a mobile phone or a portable information terminal because of a demand for a thinner and lighter device body. When impact or external force is applied by dropping or squeezing a mobile device, a display using a thin glass substrate has a problem that the display itself is damaged or the image is disturbed due to deformation or the like. It was.

そこで、ディスプレイに衝撃や外力が加わることを防止するために、プラスティック製の保護板、例えば透明性の高いアクリル樹脂製の保護板をディスプレイ外側に一定の間隔を保って平行に配置している（例えば、特許文献１参照。）。   Therefore, in order to prevent an impact or external force from being applied to the display, a protective plate made of plastic, for example, a protective plate made of highly transparent acrylic resin, is arranged in parallel with a certain distance on the outside of the display ( For example, see Patent Document 1.)

しかし、アクリル樹脂製の保護板は外力によって撓みやすいとともに、ある程度の強度を得るためには厚肉にする必要であるため、装置の薄型化には限界があった。   However, since the protective plate made of acrylic resin is easily bent by an external force and needs to be thick to obtain a certain degree of strength, there is a limit to reducing the thickness of the device.

また、この保護板を長期間にわたって使用するとアクリル樹脂が劣化して透明度が損なわれる場合がある。このような問題を解決するためにアクリル樹脂の替わりに白ガラスからなる板ガラスを保護板に使用することが提案されている（例えば、特許文献２参照。）。
特開２００４−２９９１９９号公報 特開２００３−１４０５５８号公報 Moreover, when this protective plate is used over a long period of time, the acrylic resin may deteriorate and the transparency may be impaired. In order to solve such problems, it has been proposed to use a glass plate made of white glass instead of an acrylic resin as a protective plate (see, for example, Patent Document 2).
JP 2004-299199 A JP 2003-140558 A

しかし、ガラスは破損した場合、破片が飛散しやすいとともに切創の危険があるという問題を有している。そのため破損しにくいようにガラスを強化する必要があるが、反射防止等の機能を付与するために膜付けする際に強化した効果が損なわれる場合があった。   However, when glass is broken, there is a problem that fragments are easily scattered and there is a risk of cutting. Therefore, it is necessary to reinforce the glass so that it is not easily damaged, but the strengthened effect may be impaired when the film is attached to provide functions such as antireflection.

本発明の目的は、強化によって充分な大きさの圧縮応力層を有するため破損しにくく、膜付け等の処理を行なっても強化した効果が損なわれない強化ガラス物品およびその製造方法を提供することである。   An object of the present invention is to provide a tempered glass article that has a sufficiently large compressive stress layer by strengthening and is not easily damaged, and that does not impair the strengthened effect even if a treatment such as filming is performed, and a method for producing the same. It is.

本発明者等は、上記課題について鋭意検討を行なった結果、膜付けによってガラスを強化した効果が損なわれる理由は、膜付けする際に加熱されるために強化によって得られた圧縮応力が緩和されるからであるが、ガラスがＳｉＯ2、Ａｌ2Ｏ3およびＺｒＯ2の成分を多く含有し、歪点が一定の値以上であると、膜付けのための加熱処理を施しても、圧縮応力が緩和しにくいことを見いだし、本発明として提案するものである。 As a result of intensive studies on the above problems, the inventors of the present invention have the reason that the effect of strengthening the glass by filming is impaired, because the compressive stress obtained by the strengthening is alleviated because it is heated during filming. However, if the glass contains a large amount of components of SiO 2 , Al 2 O 3 and ZrO 2 and the strain point is a certain value or more, the compressive stress is applied even if the heat treatment for film formation is performed. Is found to be difficult to relax, and is proposed as the present invention.

本発明の強化ガラス物品は、歪点が５５０℃以上であって、表面より１〜１００μｍまでの深さに１００ＭＰａ以上の圧縮応力層を有することを特徴とする。   The tempered glass article of the present invention has a compressive stress layer having a strain point of 550 ° C. or higher and a depth of 1 to 100 μm from the surface of 100 MPa or higher.

また、本発明の強化ガラス物品の製造方法は、質量％表示で、ＳｉＯ2＋Ａｌ2Ｏ3＋ＺｒＯ2 ６０〜８０％、ＭｇＯ＋ＣａＯ＋ＳｒＯ＋ＢａＯ １０〜３０％、Ｌｉ2Ｏ＋Ｎａ2Ｏ ０．５〜１５％の組成を含有する板ガラスを、硝酸カリウムを含有する４００℃〜５５０℃の融液中に１〜４８時間浸漬することを特徴とする。 A method of manufacturing a tempered glass article of the present invention, represented by mass%, SiO 2 + Al 2 O 3 + ZrO 2 60~80%, MgO + CaO + SrO + BaO 10~30%, Li 2 O + Na 2 O 0.5~15% of the composition The plate glass containing is immersed in a 400 ° C to 550 ° C melt containing potassium nitrate for 1 to 48 hours.

本発明の強化ガラス物品は、強化によって充分な大きさの圧縮応力層を有するため破損しにくく、しかも歪点が高いため膜付け等の加熱処理を行なっても圧縮応力が緩和しにくく強化した効果が損なわれにくい。   The tempered glass article of the present invention has a compressive stress layer having a sufficiently large size due to strengthening, and it is difficult to break, and since the strain point is high, the compressive stress is hardly relaxed even if heat treatment such as filming is performed, and the strengthened effect Is hard to be damaged.

本発明の強化ガラス物品は、歪点が５５０℃以上であるため、強化後に膜付け等の加熱処理を行なっても強化された効果が損なわれにくいが、歪点が５７０℃以上であるとより好ましく、５８０℃以上であるとさらに好ましい。   Since the tempered glass article of the present invention has a strain point of 550 ° C. or higher, the strengthened effect is hardly impaired even if heat treatment such as filming is performed after tempering, but the strain point is more than 570 ° C. Preferably, it is more preferably 580 ° C. or higher.

また、強化によって１００ＭＰａ以上の圧縮応力層が形成されているため破損しにくいが、２００ＭＰａ以上の圧縮応力層が形成されているとより好ましく、３００ＭＰａ以上であるとさらに好ましい。   Moreover, although the compressive stress layer of 100 MPa or more is formed by strengthening, it is difficult to break, but it is more preferable that a compressive stress layer of 200 MPa or more is formed, and further more preferable that it is 300 MPa or more.

また、軽量化のため密度は２．９ｇ／ｃｍ3以下であると好ましく、２．８ｇ／ｃｍ3以下であるとより好ましく、２．７ｇ／ｃｍ3以下であるとさらに好ましい。 In order to reduce the weight, the density is preferably 2.9 g / cm 3 or less, more preferably 2.8 g / cm 3 or less, and even more preferably 2.7 g / cm 3 or less.

上記した特性を満たすガラスは、例えば質量％表示で、ＳｉＯ2＋Ａｌ2Ｏ3＋ＺｒＯ2 ６０〜８０％、ＭｇＯ＋ＣａＯ＋ＳｒＯ＋ＢａＯ １０〜３０％、Ｌｉ2Ｏ＋Ｎａ2Ｏ ０．５〜１５％の組成を含有し、風冷強化（物理強化）またはアルカリ金属イオンのイオン交換による化学強化が行なわれて作製される。このように組成範囲を決定した理由を以下に述べる。なお、以下の説明で、特に断りがない限り"％"は"質量％"を意味する。 The glass satisfying the above-mentioned characteristics contains, for example, a composition of SiO 2 + Al 2 O 3 + ZrO 2 60 to 80%, MgO + CaO + SrO + BaO 10 to 30%, Li 2 O + Na 2 O 0.5 to 15% in terms of mass%. It is produced by air-cooling strengthening (physical strengthening) or chemical strengthening by ion exchange of alkali metal ions. The reason for determining the composition range in this way will be described below. In the following description, “%” means “mass%” unless otherwise specified.

ＳｉＯ2、Ａｌ2Ｏ3およびＺｒＯ2は、歪点を高める成分であり、その合量が６０％よりも少ないと充分に歪点を高めることができず、８０％よりも多いとガラスの高温粘度が高くなるとともに未溶解物が発生しやすくなるため好ましくない。これらの成分の合量が６２〜７８％であると好ましく、６５〜７５％であるとより好ましい。 SiO 2 , Al 2 O 3 and ZrO 2 are components that increase the strain point. When the total amount is less than 60%, the strain point cannot be sufficiently increased, and when it exceeds 80%, the glass has a high temperature. This is not preferable because the viscosity increases and undissolved substances are easily generated. The total amount of these components is preferably 62 to 78%, and more preferably 65 to 75%.

ＳｉＯ2の含有量は、５０〜７５％であると好ましい。ＳｉＯ2の含有量が７５％よりも多くなると、ガラスの高温粘度が高くなり溶融しにくくなるとともに、液相温度が上昇するため、成形が難しくなったり、失透が発生しやすくなったりする傾向がある。一方、含有量が５０％よりも少なくなると、密度が大きくなりガラス物品の質量が大きくなる傾向がある。ＳｉＯ2の含有量は５１〜７０％であると好ましく、５２〜６８％であるとより好ましく、５３〜６５％であるとさらに好ましく、５４〜６０％であると最も好ましい。 The content of SiO 2 is preferably 50 to 75%. When the content of SiO 2 exceeds 75%, the high-temperature viscosity of the glass becomes high and difficult to melt, and the liquidus temperature rises, so that molding tends to be difficult or devitrification tends to occur. There is. On the other hand, when the content is less than 50%, the density tends to increase and the mass of the glass article tends to increase. The content of SiO 2 is preferably 51 to 70%, more preferably 52 to 68%, still more preferably 53 to 65%, and most preferably 54 to 60%.

Ａｌ2Ｏ3は、歪点を上昇させる効果があるとともに、化学強化をしやすくする作用を持つため本発明において必須の成分であり、０．５〜１５％含有すると好ましい。ただし含有量が１５％よりも多くなると、ガラス表面に失透結晶が析出しやすくなったり、ガラスの高温粘度が高くなったり、溶融、成形が難しくなったりする傾向がある。一方、０．５％よりも少ないと、上記した効果が得られにくい。Ａｌ2Ｏ3の含有量は１〜１３％であると好ましく、１．５〜１２％であるとより好ましく、１．５〜１１％あることが最も好ましい。 Al 2 O 3 is an essential component in the present invention because it has the effect of increasing the strain point and facilitates chemical strengthening, and is preferably contained in an amount of 0.5 to 15%. However, if the content exceeds 15%, devitrified crystals tend to precipitate on the glass surface, the high-temperature viscosity of the glass tends to increase, and melting and molding tend to be difficult. On the other hand, if it is less than 0.5%, the above-described effects are hardly obtained. The content of Al 2 O 3 is preferably 1 to 13%, more preferably 1.5 to 12%, and most preferably 1.5 to 11%.

ＺｒＯ2は、歪点や耐候性を上昇させる成分であり、１０％まで含有することができる。ＺｒＯ2の含有量が１０％よりも多くなると、失透が発生する傾向にあり、成形が難しくなる。ＺｒＯ2の含有量は、８％以下であるとより好ましく、７％以下であるとさらに好ましい。 ZrO 2 is a component that increases the strain point and weather resistance, and can be contained up to 10%. When the content of ZrO 2 exceeds 10%, devitrification tends to occur and molding becomes difficult. The content of ZrO 2 is more preferably 8% or less, and further preferably 7% or less.

ＭｇＯ、ＣａＯ、ＳｒＯおよびＢａＯは、歪点を低下させずに高温粘性を小さくする成分であり、合量で１０〜３０％添加される。これらの成分の合量が３０％よりも多いと失透が発生する傾向があり、１０％よりも少ないと上記した効果を充分に得ることができない傾向がある。１２〜２８％であると好ましく、１３〜２６％であるとより好ましく、１４〜２４％であるとさらに好ましい。   MgO, CaO, SrO and BaO are components that reduce high temperature viscosity without lowering the strain point, and are added in a total amount of 10 to 30%. If the total amount of these components is more than 30%, devitrification tends to occur, and if it is less than 10%, the above-mentioned effects tend not to be sufficiently obtained. It is preferably 12 to 28%, more preferably 13 to 26%, and further preferably 14 to 24%.

ＭｇＯは、歪点を低下させずにガラスの高温粘度を低下させて溶融性や成形性を高める成分であり、１０％まで含有することができる。ただしＭｇＯの含有量が１０％よりも多くなると、ガラスが失透しやすくなる傾向にある。ＭｇＯの含有量が０．１〜８．５％であるとより好ましく、０．５〜８％であるとさらに好ましい。   MgO is a component that lowers the high temperature viscosity of the glass without lowering the strain point and improves the meltability and formability, and can be contained up to 10%. However, when the content of MgO exceeds 10%, the glass tends to be devitrified. The content of MgO is more preferably 0.1 to 8.5%, and further preferably 0.5 to 8%.

ＣａＯは、歪点を低下させずにガラスの高温粘度を低下させて溶融性や成形性を高める成分であり、１２％まで含有することができる。ただしＣａＯの含有量が１２％よりも多くなると、ガラスが失透しやすくなるとともに、ガラスの密度が高くなる傾向にある。ＣａＯの含有量が０．１〜９％であるとより好ましく、０．５〜６％であるとさらに好ましい。   CaO is a component that reduces the high temperature viscosity of the glass without increasing the strain point and improves the meltability and moldability, and can be contained up to 12%. However, when the content of CaO exceeds 12%, the glass tends to be devitrified and the density of the glass tends to increase. The content of CaO is more preferably 0.1 to 9%, and further preferably 0.5 to 6%.

ＳｒＯは、歪点を低下させずにガラスの高温粘度を低下させて溶融性や成形性を高める成分であり、１５％まで含有することができる。ただしＳｒＯの含有量が１５％よりも多くなると、ガラスが失透しやすくなるとともに、ガラスの密度が高くなる傾向にある。０．１〜１２％であるとより好ましく、１〜１１％であるとさらに好ましい。   SrO is a component that improves the meltability and moldability by reducing the high-temperature viscosity of the glass without reducing the strain point, and can be contained up to 15%. However, when the content of SrO exceeds 15%, the glass tends to be devitrified and the density of the glass tends to increase. More preferably, it is 0.1 to 12%, and further preferably 1 to 11%.

ＢａＯは、歪点を低下させずにガラスの高温粘度を低下させて溶融性や成形性を高める成分であり、１２％まで含有することができる。ただしＢａＯの含有量が１２％よりも多くなると、ガラスが失透しやすくなるとともに、ガラスの密度が高くなる傾向にある。ただしＢａＯの含有量が０．０５〜１０％であるとより好ましい。   BaO is a component that lowers the high temperature viscosity of the glass without lowering the strain point and improves the meltability and moldability, and can be contained up to 12%. However, when the content of BaO exceeds 12%, the glass tends to be devitrified and the density of the glass tends to increase. However, the content of BaO is more preferably 0.05 to 10%.

Ｌｉ2ＯとＮａ2Ｏは、Ｋ+とイオン交換される成分であり、これによって化学強化されて圧縮応力層が形成される。これらの成分の合量が０．５〜１５％であると好ましい。これらの成分の含有量が０．５％よりも少ないと充分に化学強化されにくく、１５％よりも多いと歪点が低くなる傾向があるため好ましくない。これらの成分の含有量が１〜１３％であるとより好ましく、１．５〜１０％であるとさらに好ましい。 Li 2 O and Na 2 O are components that are ion-exchanged with K +, and are thereby chemically strengthened to form a compressive stress layer. The total amount of these components is preferably 0.5 to 15%. If the content of these components is less than 0.5%, it is difficult to be sufficiently chemically strengthened, and if it is more than 15%, the strain point tends to be low, such being undesirable. The content of these components is more preferably 1 to 13%, and further preferably 1.5 to 10%.

Ｌｉ2Ｏは、ガラスの高温粘度を低下させて溶融性や成形性を高める成分であるとともに、イオン交換によって化学強化できる成分であり、５％まで含有することができる。Ｌｉ2Ｏの含有量が５％よりも多いとガラスが分相しやすいとともに歪点が低下しやすい。Ｌｉ2Ｏの含有量は４％以下であると好ましく、３％以下であるとより好ましい。 Li 2 O is a component that lowers the high-temperature viscosity of the glass to improve the meltability and formability, and can be chemically strengthened by ion exchange, and can be contained up to 5%. When the content of Li 2 O is more than 5%, the glass tends to phase-separate and the strain point tends to decrease. The Li 2 O content is preferably 4% or less, and more preferably 3% or less.

Ｎａ2Ｏは、ガラスの高温粘度を低下させて溶融性や成形性を高める成分であるとともに、イオン交換によって化学強化できる成分であり、１５％まで含有することができる。Ｎａ2Ｏの含有量が１５％よりも多くなるとガラスが失透しやすくなるとともに、歪点が低下する傾向にある。Ｎａ2Ｏの含有量は０．５〜１２％であると好ましく、１〜９％であるとより好ましく、１．５〜７％であるとさらに好ましい。 Na 2 O is a component that lowers the high-temperature viscosity of the glass to improve the meltability and formability, and is a component that can be chemically strengthened by ion exchange, and can be contained up to 15%. When the content of Na 2 O exceeds 15%, the glass tends to devitrify and the strain point tends to decrease. The content of Na 2 O is preferably 0.5 to 12%, more preferably 1 to 9%, and further preferably 1.5 to 7%.

本発明では、上記した成分以外にも以下の成分を添加することが可能である。   In the present invention, it is possible to add the following components in addition to the components described above.

Ｋ2Ｏは、ガラスの高温粘度を低下させて溶融性や成形性を高める成分であり、１５％まで含有することができる。Ｋ2Ｏの含有量が１５％よりも多くなると化学強化がしにくくなるとともに、ガラスが失透しやすく、歪点も低下する傾向にある。Ｋ2Ｏの含有量は０．１〜１２％であると好ましく、０．５〜９％であるとより好ましく、１〜８％であるとさらに好ましい。 K 2 O is a component that lowers the high-temperature viscosity of the glass and improves the meltability and moldability, and can be contained up to 15%. When the content of K 2 O exceeds 15%, chemical strengthening becomes difficult, the glass tends to devitrify, and the strain point tends to decrease. The content of K 2 O is preferably 0.1 to 12%, more preferably 0.5 to 9%, and further preferably 1 to 8%.

Ｐ2Ｏ5は、失透の発生を抑制する成分であり５％まで添加することができる。Ｐ2Ｏ5の含有量が５％よりも多くなるとガラスが分相しやすくなる。Ｐ2Ｏ5の含有量は４％以下であると好ましく、３％以下であるとより好ましい。 P 2 O 5 is a component that suppresses the occurrence of devitrification, and can be added up to 5%. When the content of P 2 O 5 is more than 5%, the glass is likely to undergo phase separation. The content of P 2 O 5 is preferably 4% or less, and more preferably 3% or less.

また、Ｂ2Ｏ3、ＺｎＯおよびＴｉＯ2の成分から選択された１種または２種以上を５％まで添加することが可能である。また、清澄剤としてＳＯ3、Ｓｂ2Ｏ3、Ｓｂ2Ｏ5、Ｃｌ、ＦおよびＳｎＯ2の群から選択された１種または２種以上を０〜３％含有させてもよい。また、Ｌａ2Ｏ3、Ｙ2Ｏ3、Ｎｂ2Ｏ5等の元素についても５％以下の範囲で含有させることができる。これらの元素はガラスの液相粘度を上げ、本発明のガラスをより製造しやすくするために役立つ。またＦｅ2Ｏ3、ＣｕＯ、ＭｎＯ2などの着色元素はガラスの透過率を低下させるので、好ましくは１％以下、より好ましくは０．５％以下に制限すべきである。 Further, it is possible to add up to 5% of one or more selected from B 2 O 3 , ZnO and TiO 2 components. Further, SO 3, Sb 2 O 3 , Sb 2 O 5, Cl, 1 kind selected from a group of F and SnO 2 or two or more may be contained 0-3% as a fining agent. Further, elements such as La 2 O 3 , Y 2 O 3 , and Nb 2 O 5 can be contained in a range of 5% or less. These elements serve to increase the liquid phase viscosity of the glass and make it easier to produce the glass of the present invention. Further, since coloring elements such as Fe 2 O 3 , CuO, and MnO 2 reduce the transmittance of the glass, they should preferably be limited to 1% or less, more preferably 0.5% or less.

本発明の強化ガラス物品は、液相温度が１１５０℃以下であると、０．７ｍｍ以下の薄い板ガラスや複雑な形状に成形しやすいため好ましい。液相温度は１１３０℃以下であると好ましく、１１００℃以下であるとより好ましい。   The tempered glass article of the present invention preferably has a liquidus temperature of 1150 ° C. or lower because it can be easily formed into a thin plate glass of 0.7 mm or less or a complicated shape. The liquidus temperature is preferably 1130 ° C. or lower, and more preferably 1100 ° C. or lower.

また、液相温度におけるガラスの粘度が高い程、素材ガラスの成形が容易になるため有利であり、１０4.0ｄＰａ・ｓ以上、１０4.3ｄＰａ・ｓ以上であると好ましく、１０4.5ｄＰａ・ｓ以上であるとより好ましく、１０4.7ｄＰａ・ｓ以上であるとさらに好ましく、１０5.0ｄＰａ・ｓ以上であると最も好ましい。 Further, the higher the viscosity of the glass at the liquidus temperature, the easier it is to form the material glass, which is advantageous. It is preferably 10 4.0 dPa · s or more, preferably 10 4.3 dPa · s or more, and 10 4.5 dPa · s or more. More preferably, it is more preferably 10 4.7 dPa · s or more, and most preferably 10 5.0 dPa · s or more.

また、本発明の強化ガラス物品は、ヤング率が大きいほどたわみにくいため携帯機器等の薄型化できるため好ましい。具体的にヤング率は７５ＧＰａ以上であると好ましく、８０ＧＰａ以上であるとより好ましい。   In addition, the tempered glass article of the present invention is preferable because the larger Young's modulus is, the more difficult it is to bend. Specifically, the Young's modulus is preferably 75 GPa or more, and more preferably 80 GPa or more.

本発明の強化ガラス物品は、携帯機器のディスプレイ等の保護板として使用する場合、その表面に各種機能性膜、特に無機材料の膜を含む機能性膜が形成されていると好ましい。   When the tempered glass article of the present invention is used as a protective plate for a display of a portable device, it is preferable that various functional films, particularly a functional film including an inorganic material film, be formed on the surface thereof.

特に、反射防止膜が形成されていると、ディスプレイの表示が見やすいため好ましい。反射防止膜としては酸化物膜や窒化物膜からなる多層膜が使用可能である。   In particular, it is preferable that an antireflection film is formed because the display on the display is easy to see. A multilayer film made of an oxide film or a nitride film can be used as the antireflection film.

膜付けには、ＣＶＤ法、ＰＶＤ法、スパッタ法、ディップ法等が可能であるが、スパッタ法は、緻密で密着性の高い膜を形成できるため好ましい。   The film can be formed by CVD, PVD, sputtering, dipping, or the like, but sputtering is preferable because a dense and highly adhesive film can be formed.

本発明の強化ガラス物品は、透明導電膜が形成されてなると電磁波を遮蔽できるとともに、帯電しにくくほこりなどが付着しにくいため好ましい。透明導電膜としてはスズ含有酸化インジウム（ＩＴＯ）、アンチモン含有酸化インジウム、フッ素含有酸化インジウム等の酸化物やアルミニウム、金、銀等の金属薄膜が使用可能である。またこれらの無機膜を用いて基板表面にタッチパネルなどの機能を持たせることも十分に可能である。   The tempered glass article of the present invention is preferably formed with a transparent conductive film because it can shield electromagnetic waves and is difficult to be charged and dust and the like are not easily adhered. As the transparent conductive film, oxides such as tin-containing indium oxide (ITO), antimony-containing indium oxide, and fluorine-containing indium oxide, and metal thin films such as aluminum, gold, and silver can be used. It is also possible to give these substrates a function such as a touch panel using these inorganic films.

また、本発明の強化ガラス部品を携帯機器の保護板として使用する場合、フロート法やダウンドロー法（スロットダウンドロー法、オーバーフローダウンドロー法等）などの成形法で得られた板ガラスの他、例えばインゴットから切り出した板状ガラスや、プレス成形された板状やその他の形状のガラスなどを用いることができる。   In addition, when the tempered glass component of the present invention is used as a protective plate for a portable device, in addition to plate glass obtained by a molding method such as a float method or a down draw method (slot down draw method, overflow down draw method, etc.) It is possible to use plate-like glass cut out from an ingot, press-molded plate-like glass or other shapes.

以下、本発明の強化ガラス物品の製造方法を説明する。   Hereinafter, the manufacturing method of the tempered glass article of the present invention is explained.

まず、所定のガラス組成となるようにガラス原料を調合し、ガラス原料を溶融炉で溶融した後、溶融ガラスから所定の形状のガラス物品を作製する。ガラス物品の作製方法には、フロート法、ロール法、またはオーバーフローダウンドロー法やスロットダウン法に代表されるダウンドロー法、プレス成形法、インゴットからの切り出し法等が使用可能である。特に、板状の場合、フロート法やダウンドロー法は表面品位が高く連続生産可能であるため好ましい。必要に応じて端面加工や光学研摩してもよい。   First, a glass raw material is prepared so as to have a predetermined glass composition, and after melting the glass raw material in a melting furnace, a glass article having a predetermined shape is produced from the molten glass. As a method for producing a glass article, a float method, a roll method, a down draw method represented by an overflow down draw method or a slot down method, a press molding method, a cutting method from an ingot, or the like can be used. In particular, in the case of a plate shape, the float method and the downdraw method are preferable because the surface quality is high and continuous production is possible. End face processing and optical polishing may be performed as necessary.

最後に、４００〜５５０℃の硝酸カリウム融液に板ガラスを１〜４８時間浸漬して強化ガラス物品を作製する。その後、必要に応じて、反射防止膜、透明導電膜、飛散防止膜等の機能性膜を表面に形成してもよい。   Finally, a plate glass is immersed in a 400 to 550 ° C. potassium nitrate melt for 1 to 48 hours to produce a tempered glass article. Thereafter, if necessary, a functional film such as an antireflection film, a transparent conductive film, or a scattering prevention film may be formed on the surface.

表１は、実施例の組成および特性を示す。   Table 1 shows the compositions and properties of the examples.

表１に示す実施例は、以下のようにして作製した。   Examples shown in Table 1 were produced as follows.

まず、表１に記載の組成となるようにそれぞれガラス原料を調合し、白金ポットを用いて１６００℃で４時間溶融した。つづいて、溶融ガラスをカーボン板の上に流し出して板状に成形して作製した。   First, each glass raw material was prepared so that it might become a composition of Table 1, and it melted at 1600 degreeC for 4 hours using the platinum pot. Subsequently, the molten glass was cast on a carbon plate and formed into a plate shape.

密度は、周知のアルキメデス法によって測定した。   The density was measured by the well-known Archimedes method.

熱膨張係数は、ディラトメーターを用いて、３０〜３８０℃における平均熱膨張係数を測定したものである。   The thermal expansion coefficient is an average thermal expansion coefficient measured at 30 to 380 ° C. using a dilatometer.

歪点および徐冷点は、ＡＳＴＭ Ｃ３３６−７１の方法に基づいて測定した。なお、この値が高いほど、強化ガラスに加わった圧縮応力が、膜付け等の各種処理によって緩和しにくいことを示す。   The strain point and annealing point were measured based on the method of ASTM C336-71. In addition, it shows that the higher this value is, the more difficult it is to relax the compressive stress applied to the tempered glass by various treatments such as film deposition.

軟化点は、ＡＳＴＭ Ｃ３３８−９３の方法に基づいて測定を行った。   The softening point was measured based on the method of ASTM C338-93.

粘度が、１０4.0ｄＰａ・ｓ、１０3.0ｄＰａ・ｓおよび１０2.5ｄＰａ・ｓにおける温度を、白金球引き上げ法で測定した。なお、これらの温度が低いほど、溶融性に優れていることになる。 Temperatures at viscosities of 10 4.0 dPa · s, 10 3.0 dPa · s, and 10 2.5 dPa · s were measured by a platinum ball pulling method. Note that the lower the temperature, the better the meltability.

液相温度は、実施例の板ガラスを粉砕し、標準篩３０メッシュ（５００μｍ）を通過し、５０メッシュ（３００μｍ）に残るガラス粉末を白金ボートに入れ、温度勾配炉中に２４時間保持して、結晶の析出する最も高い温度を測定したものである。   The liquid phase temperature is obtained by crushing the plate glass of the example, passing through a standard sieve 30 mesh (500 μm), putting the glass powder remaining in 50 mesh (300 μm) into a platinum boat, and holding it in a temperature gradient furnace for 24 hours. The highest temperature at which crystals precipitate is measured.

また、液相粘度は、液相温度における各試料の粘度を示す。液相粘度が高く、液相温度が低いほど、耐失透性に優れ、成形性に優れているといえる。   Moreover, liquid phase viscosity shows the viscosity of each sample in liquid phase temperature. The higher the liquidus viscosity and the lower the liquidus temperature, the better the devitrification resistance and the better the moldability.

また、以下の方法で実施例の板ガラスを化学強化し、評価した。   Moreover, the plate glass of an Example was chemically strengthened and evaluated by the following methods.

まず、実施例の板ガラスを、ダウンドロー法で厚さ０．７ｍｍに成形した。これを３５ｍｍ×３５ｍｍのサイズに切断し、端面を面取りした。基板両面の表面は酸化セリウムを用いて鏡面研磨を施した。   First, the plate glass of an Example was shape | molded by thickness 0.7mm by the down draw method. This was cut into a size of 35 mm × 35 mm, and the end face was chamfered. The surfaces on both sides of the substrate were mirror-polished using cerium oxide.

次に、この板ガラスを４７０℃の硝酸カリウム融液に４時間浸漬して強化ガラスの試料を作製した。   Next, this plate glass was immersed in a potassium nitrate melt at 470 ° C. for 4 hours to prepare a sample of tempered glass.

この試料の表面の圧縮応力層の圧縮応力値および応力層深さを応力計（東芝製表面応力計ＦＳＭ−６０）を用いて測定した。   The compressive stress value and the stress layer depth of the compressive stress layer on the surface of this sample were measured using a stress meter (Toshiba surface stress meter FSM-60).

そして、強化前のガラスおよび強化後のガラスを内径φ２５ｍｍの平滑なステンレス（ＳＵＳ３０４）製のリング上に置き、上部中央よりφ１２．５ｍｍの平滑な面で破損するまで荷重を加えて破壊応力を測定し、５回の平均値（平均破壊応力）を算出した。   The glass before strengthening and the glass after strengthening are placed on a smooth stainless steel (SUS304) ring with an inner diameter of φ25 mm, and the fracture stress is measured by applying a load from the upper center until it breaks on a smooth surface with φ12.5 mm. And the average value (average fracture stress) of 5 times was calculated.

表１から明らかなように、実施例の板ガラスはイオン交換によって充分に強化することができ、歪点が充分に高かった。このため、各種機能成膜を成膜しても成膜の際に強化した効果は損なわれないものと考えられる。   As is apparent from Table 1, the plate glass of the example could be sufficiently strengthened by ion exchange and had a sufficiently high strain point. For this reason, it is considered that even if various types of functional film are formed, the enhanced effect is not impaired.

本発明の強化ガラス物品は、薄肉、軽量、高強度であり、耐熱性にも優れ、各種の薄膜を形成しやすいことから、携帯電話、携帯情報端末（ＰＤＡ）、デジタルカメラ以外にも、携帯用ゲーム機、ポータブル音楽プレイヤー、電子時辞書等のディスプレイの保護板として好適である。また、ディスプレイに限らず、携帯機器の例えばレンズカバーやスケルトンタイプのカバー部材等にも使用可能である。   The tempered glass article of the present invention is thin, lightweight, high-strength, excellent in heat resistance, and easy to form various thin films. Therefore, the tempered glass article is not limited to mobile phones, personal digital assistants (PDAs), and digital cameras. It is suitable as a protective plate for displays of game machines, portable music players, electronic dictionaries and the like. Further, the present invention can be used not only for a display but also for a portable device such as a lens cover or a skeleton type cover member.

Claims (8)

歪点が５５０℃以上であって、表面より１〜１００μｍまでの深さに１００ＭＰａ以上の圧縮応力層を有することを特徴とする強化ガラス物品。   A tempered glass article having a compressive stress layer having a strain point of 550 ° C. or more and a depth of 1 to 100 μm from the surface of 100 MPa or more. 質量％表示で、ＳｉＯ2＋Ａｌ2Ｏ3＋ＺｒＯ2 ６０〜８０％、ＭｇＯ＋ＣａＯ＋ＳｒＯ＋ＢａＯ １０〜３０％、Ｌｉ2Ｏ＋Ｎａ2Ｏ ０．５〜１５％の組成を含有することを特徴とする請求項１に記載の強化ガラス物品。 2. The composition according to claim 1, comprising a composition of SiO 2 + Al 2 O 3 + ZrO 2 60 to 80%, MgO + CaO + SrO + BaO 10 to 30%, Li 2 O + Na 2 O 0.5 to 15% by mass%. Tempered glass articles. 液相温度が１１５０℃以下であることを特徴とする請求項１または２に記載の強化ガラス物品。   Liquid phase temperature is 1150 degrees C or less, The tempered glass article of Claim 1 or 2 characterized by the above-mentioned. 圧縮応力層が化学強化によって形成されてなることを特徴とする請求項１〜３のいずれかに記載の強化ガラス物品。   The tempered glass article according to claim 1, wherein the compressive stress layer is formed by chemical strengthening. 機能性膜が形成されていることを特徴とする請求項１〜４に記載の強化ガラス物品。   The tempered glass article according to claim 1, wherein a functional film is formed. 請求項１〜５に記載の強化ガラス物品を、保護板として使用してなることを特徴とする携帯機器。   A portable device comprising the tempered glass article according to claim 1 as a protective plate. 質量％表示で、ＳｉＯ2＋Ａｌ2Ｏ3＋ＺｒＯ2 ６０〜８０％、ＭｇＯ＋ＣａＯ＋ＳｒＯ＋ＢａＯ １０〜３０％、Ｌｉ2Ｏ＋Ｎａ2Ｏ ０．５〜１５％の組成を含有する板ガラスを、硝酸カリウムを含有する４００℃〜５５０℃の融液中に１〜４８時間浸漬することを特徴とする強化ガラス物品の製造方法。 A plate glass containing a composition of SiO 2 + Al 2 O 3 + ZrO 2 60 to 80%, MgO + CaO + SrO + BaO 10 to 30%, Li 2 O + Na 2 O 0.5 to 15% by mass%, 400 ° C. containing potassium nitrate A method for producing a tempered glass article comprising immersing in a melt at 550 ° C. for 1 to 48 hours. フロート法またはダウンドロー法により成形された板ガラスを用いることを特徴とする請求項７に記載の強化ガラス物品の製造方法。   The method for producing a tempered glass article according to claim 7, wherein a plate glass formed by a float process or a downdraw process is used.
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CN113165969B (en) * 2018-12-11 2023-04-04 Ａｇｃ株式会社 Chemically strengthened glass plate, cover glass comprising chemically strengthened glass, and electronic device
CN113165969A (en) * 2018-12-11 2021-07-23 Ａｇｃ株式会社 Chemically strengthened glass plate, cover glass comprising chemically strengthened glass, and electronic device

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