JP2011057547A - Glass substrate for display, method for producing the same, and display using the same - Google Patents
Glass substrate for display, method for producing the same, and display using the same Download PDFInfo
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本発明はディスプレイ用のガラス基板及びその製造方法並びにこれを用いたディスプレイに関する。 The present invention relates to a glass substrate for display, a method for producing the same, and a display using the same.
パーソナルコンピュータや携帯電話といった情報端末の表示装置としては液晶ディスプレイが用いられている。一般に、液晶ディスプレイは透明電極が形成された１対の基板間に液晶が封入された構造を有している。この基板としてはソーダライムガラスや無アルカリガラス等で形成されたガラス基板が用いられている。 Liquid crystal displays are used as display devices for information terminals such as personal computers and mobile phones. In general, a liquid crystal display has a structure in which liquid crystal is sealed between a pair of substrates on which transparent electrodes are formed. As this substrate, a glass substrate formed of soda lime glass or non-alkali glass is used.
ところで、携帯電話、モバイル型パーソナルコンピュータ、携帯型ＡＶ機器等の携帯型情報端末といった情報端末の小型化に伴い、情報端末で使用されるディスプレイ用のガラス基板の軽量化と省電力化が要望されている。例えば、バックライトを用いずに、画像を背面に配置された反射板で反射して表示する反射型液晶ディスプレイでは、ガラス基板が厚くなると視差が生じ、画像が２重にみえ、これによって２つの画像が色をうち消しあうため、画像の輝度が低下してしまう。従って、このような液晶ディスプレイに用いられるガラス基板は特に厚さを薄くすることが重要である。 By the way, with the miniaturization of information terminals such as portable information terminals such as mobile phones, mobile personal computers, and portable AV devices, there is a demand for lightening and power saving of glass substrates for displays used in information terminals. ing. For example, in a reflective liquid crystal display in which an image is reflected and displayed by a reflector disposed on the back without using a backlight, parallax occurs when the glass substrate is thick, and the image looks double. Since the image erases the color, the brightness of the image decreases. Accordingly, it is important to reduce the thickness of the glass substrate used in such a liquid crystal display.
一方、ガラス基板は厚さが薄くなると、ディスプレイの製造工程中あるいは使用中に割れやすくなるといった問題がある。この問題に対処するため、ディスプレイ用基板として、強化処理により強度が増大された強化ガラス基板を用いることが提案されている。例えば、特開昭５７−２０５３４３号や特開平９−２３６７９２号は強化処理により強度が強化された液晶ディスプレイ用のガラス基板が開示されている。 On the other hand, when the thickness of the glass substrate is reduced, there is a problem that it is easily broken during the manufacturing process or use of the display. In order to cope with this problem, it has been proposed to use a tempered glass substrate whose strength has been increased by a tempering treatment as a display substrate. For example, Japanese Patent Application Laid-Open Nos. 57-205343 and 9-236792 disclose glass substrates for liquid crystal displays whose strength is enhanced by a strengthening treatment.
しかし、上述したガラス基板では携帯型情報端末で用いられる厚さに形成した場合、強度が十分でない場合がある。例えば、上述した反射型液晶ディスプレイでは、ディスプレイの輝度を維持するため、ガラス基板としては厚さが０．７ｍｍ以下、通常０．４ｍｍ程度のものを用いる必要がある。この場合、従来の強化ガラス基板では強化対象のガラス基板の厚さが薄いため、必要な強度を得ることが困難な場合がある。 However, when the glass substrate described above is formed to a thickness used in a portable information terminal, the strength may not be sufficient. For example, in the reflective liquid crystal display described above, in order to maintain the brightness of the display, it is necessary to use a glass substrate having a thickness of 0.7 mm or less, usually about 0.4 mm. In this case, in the conventional tempered glass substrate, since the glass substrate to be tempered is thin, it may be difficult to obtain a required strength.
また、従来の強化方法で必要な強度を持たせようとすると強化処理に長時間を要する場合がある。例えば、ソーダライムガラスで形成されたガラス基板に、厚さ５０μｍ以上の圧縮応力層を形成するためにはガラス基板を溶融塩中に１６時間以上浸漬する必要があり、たとえ必要な強度を得られたとしても製造の手間及びコストが増大してしまう。 In addition, if an attempt is made to provide the necessary strength with the conventional strengthening method, the strengthening process may take a long time. For example, in order to form a compressive stress layer having a thickness of 50 μm or more on a glass substrate formed of soda lime glass, it is necessary to immerse the glass substrate in molten salt for 16 hours or more, and the required strength can be obtained. Even if this is the case, the labor and cost of manufacturing increase.
また、強化処理に使用する処理塩によっては、ガラス基板が着色してしまったり、処理塩コストが高くなりすぎるといった問題もある。本発明は上述した問題点を解決するためになされたものであり、薄型化、軽量化が可能で、機械的強度や透明性が高く、しかも短時間で製造可能なディスプレイ用ガラス基板及びその製造方法並びにこれを用いたディスプレイを提供することを目的とする。 Further, depending on the treatment salt used for the strengthening treatment, there is a problem that the glass substrate is colored or the treatment salt cost becomes too high. The present invention has been made to solve the above-described problems, and can be reduced in thickness and weight, has high mechanical strength and transparency, and can be manufactured in a short time. It is an object to provide a method and a display using the method.
本発明は、厚さが０．７ｍｍ以下で、表面に深さ５０μｍ以上の圧縮応力層を有するディスプレイ用ガラス基板である。本発明のディスプレイ用ガラス基板は厚さが０．７ｍｍ以下と薄いため、ディスプレイの薄型化及び軽量化を図ることができると共に、ディスプレイの輝度の低下を防止することができる。また、表面に深さ５０μｍ以上の圧縮応力層を有しているため、基板の厚さが０．７ｍｍ以下であっても充分な強度を有する。例えば、本発明のガラス基板の厚さが０．４ｍｍである場合、厚さが０．８ｍｍであって圧縮応力層が形成されていないガラス基板と同等の強度を有する。本発明のディスプレイ用ガラス基板の厚さは０．２〜０．５ｍｍが好ましく、０．２〜０．４５ｍｍがより好ましく、０．２〜０．４ｍｍが最も好ましい。また、圧縮応力層の深さは７０μｍ以上が好ましく、１００μｍ以上がより好ましい。本発明に係るガラス基板の圧縮応力層の深さの上限は基板の厚さ等の条件により異なるが、通常、基板の厚さの１／４倍程度とすることが好ましい。 The present invention is a glass substrate for display having a compressive stress layer having a thickness of 0.7 mm or less and a depth of 50 μm or more on the surface. Since the glass substrate for display of the present invention is as thin as 0.7 mm or less, the display can be reduced in thickness and weight, and the luminance of the display can be prevented from being lowered. Further, since the surface has a compressive stress layer having a depth of 50 μm or more, it has sufficient strength even if the thickness of the substrate is 0.7 mm or less. For example, when the thickness of the glass substrate of the present invention is 0.4 mm, the glass substrate has a strength equivalent to that of a glass substrate having a thickness of 0.8 mm and no compression stress layer formed thereon. The thickness of the glass substrate for display of the present invention is preferably 0.2 to 0.5 mm, more preferably 0.2 to 0.45 mm, and most preferably 0.2 to 0.4 mm. Further, the depth of the compressive stress layer is preferably 70 μm or more, and more preferably 100 μm or more. Although the upper limit of the depth of the compressive stress layer of the glass substrate according to the present invention varies depending on conditions such as the thickness of the substrate, it is usually preferable to set it to about 1/4 times the thickness of the substrate.
以上の説明から明らかなように、本発明によれば、厚さを薄くしても十分な強度を有するディスプレイ用ガラス基板が提供される。従って、このような基板を用いることにより、ディスプレイの薄型化及び軽量化を図ることができると共に、消費電力を増大させることなくディスプレイの輝度の低下を防止することが可能になる。 As is clear from the above description, according to the present invention, a glass substrate for display having sufficient strength even if the thickness is reduced is provided. Therefore, by using such a substrate, it is possible to reduce the thickness and weight of the display, and it is possible to prevent the brightness of the display from decreasing without increasing the power consumption.
このような圧縮応力層はガラス基板に焼入れといった物理強化処理又はイオン交換といった化学強化処理を施すことにより形成することができる。本発明では、化学強化処理により機械的強度の高い圧縮応力層が得られること、厚さが０．７ｍｍ以下のガラス基板には物理強化処理は適さないことから化学強化処理を用いることが好ましい。 Such a compressive stress layer can be formed by subjecting a glass substrate to a physical strengthening process such as quenching or a chemical strengthening process such as ion exchange. In the present invention, it is preferable to use a chemical strengthening treatment because a compressive stress layer having high mechanical strength can be obtained by the chemical strengthening treatment and a physical strengthening treatment is not suitable for a glass substrate having a thickness of 0.7 mm or less.
この化学強化処理は、ガラス基板の表面のイオン半径が小さいアルカリイオン（例えば、ナトリウムイオン）をイオン半径の大きなアルカリイオン（例えば、カリウムイオン）に置換すること、例えば、ナトリウムイオンを含有するガラス基板をカリウムイオンを含む溶融処理塩で処理することにより行うことができる。このようなイオン交換処理が行われることにより、ガラス基板表面の圧縮応力層の組成はイオン交換処理前の組成と若干異なるが、基板深層部の組成はイオン交換処理前の組成とほぼ同じである。 In this chemical strengthening treatment, alkali ions having a small ionic radius (for example, sodium ions) on the surface of the glass substrate are replaced with alkali ions having a large ionic radius (for example, potassium ions), for example, glass substrates containing sodium ions. Can be performed by treating with a molten salt containing potassium ions. By performing such an ion exchange treatment, the composition of the compressive stress layer on the surface of the glass substrate is slightly different from the composition before the ion exchange treatment, but the composition of the deep substrate portion is almost the same as the composition before the ion exchange treatment. .
化学強化処理により圧縮応力層が形成されたかは、ガラス基板の表面付近に含まれる金属イオンの分布を調べることにより判定することができる。具体的には、イオン半径の大きなアルカリ金属イオンと、イオン半径の小さなアルカリ金属イオンの深さ分布を調べ、（イオン半径の大きな金属イオンの密度）／（イオン半径の小さな金属イオンの密度）が、ガラスの深層部（ガラスの厚みの半分の深さの部分）よりも表面に近い部分のほうが大きければ、イオン交換による化学強化が行なわれたものであることが判る。 Whether the compressive stress layer has been formed by the chemical strengthening treatment can be determined by examining the distribution of metal ions contained in the vicinity of the surface of the glass substrate. Specifically, the depth distribution of alkali metal ions with large ionic radii and alkali metal ions with small ionic radii is investigated, and (density of metal ions with large ionic radius) / (density of metal ions with small ionic radius) is If the portion closer to the surface is larger than the deep portion of the glass (the portion having a depth half the thickness of the glass), it can be understood that chemical strengthening by ion exchange has been performed.
また、圧縮応力層の深さは、精密歪み計を用いたバビネ補正法又は偏光顕微鏡を用いる方法などで求めることができる。精密歪み計を用いたバビネ補正法は市販の測定装置により行うことができる。偏光顕微鏡を用いる方法は、ガラス基板のイオン交換処理面を垂直に切断し、その断面を厚さ０．５ｍｍ以下となるよう薄く研磨した後、偏光顕微鏡にて研磨面に垂直に偏光を入射し直行ニコルにて観察することにより行うことができる。化学強化ガラスは、表面付近に圧縮応力層が形成されるため、表面から明るさや色の変化している部分の距離を測定することによって圧縮応力層の厚さが測定される。 The depth of the compressive stress layer can be determined by a Babinet correction method using a precision strain meter, a method using a polarization microscope, or the like. The Babinet correction method using a precision strain meter can be performed with a commercially available measuring device. In the method using a polarizing microscope, the ion-exchanged surface of the glass substrate is cut vertically, the cross section is thinly polished to a thickness of 0.5 mm or less, and then polarized light is incident on the polishing surface vertically with a polarizing microscope. This can be done by observing with direct Nicols. Since the chemically stressed glass has a compressive stress layer formed near the surface, the thickness of the compressive stress layer is measured by measuring the distance from the surface where the brightness or color changes.
このような化学強化処理が行われるガラス基板としては、イオン半径の小さなアルカリイオン（例えば、カリウム以下のアルカリ金属イオン）を含有するガラス基板が用いられる。また、圧縮応力層を形成するためには、ガラス基板が歪み点以下のときに溶融処理塩で処理する必要があるため、歪み点が一定温度以上のガラス基板が用いられる。 As the glass substrate on which such chemical strengthening treatment is performed, a glass substrate containing alkali ions having a small ionic radius (for example, alkali metal ions of potassium or less) is used. Moreover, in order to form a compressive stress layer, since it is necessary to process with a molten process salt when a glass substrate is below a strain point, the glass substrate with a strain point more than fixed temperature is used.
このようなガラス基板の組成は、耐久性、安定性、イオン交換効率、歪み点、透明性、溶解性、機械強度等を考慮して定めることができるが、ＳｉＯ2、Ａｌ2Ｏ3、Ｌｉ2Ｏ、Ｎａ2Ｏ及びＺｒＯ2を含むことが好ましい。上記成分の含有量については以下の点を考慮して決められる。 The composition of such a glass substrate can be determined in consideration of durability, stability, ion exchange efficiency, strain point, transparency, solubility, mechanical strength, etc., but SiO 2 , Al 2 O 3 , Li Preferably, it contains 2 O, Na 2 O and ZrO 2 . The content of the above components is determined in consideration of the following points.
ＳｉＯ2はガラス骨格を形成する必須成分であり、その含有量が４０重量％未満であると化学的耐久性が悪化し、逆に７０重量％を超えると溶融温度が高くなりすぎる。従って、ＳｉＯ2の含有量は４０〜７０重量％とすることが好ましい。 SiO 2 is an essential component for forming a glass skeleton. When the content is less than 40% by weight, the chemical durability is deteriorated. On the other hand, when it exceeds 70% by weight, the melting temperature becomes too high. Accordingly, the content of SiO 2 is preferably 40 to 70% by weight.
Ａｌ2Ｏ3はガラス表面のイオン交換性能を向上させる成分であり、その含有量が０．１重量％未満であるとその効果がなく、逆に２０重量％を超えると耐失透性が低下する。従って、Ａｌ2Ｏ3含有量は０．１〜２０重量％とすることが好ましい。 Al 2 O 3 is a component that improves the ion exchange performance of the glass surface. If its content is less than 0.1% by weight, it will not be effective, and conversely if it exceeds 20% by weight, devitrification resistance will decrease. To do. Accordingly, the Al 2 O 3 content is preferably 0.1 to 20% by weight.
Ｎａ2Ｏはイオン交換処理において主としてカリウムイオンと置換されることによってガラスを化学強化する成分であり、その含有量が２０重量％を越える化学的耐久性が低下する。従って、Ｎａ2Ｏの含有量は０〜２０重量％とすることが好ましい。 Na 2 O is a component that chemically strengthens the glass by being mainly replaced with potassium ions in the ion exchange treatment, and the chemical durability of which the content exceeds 20% by weight is lowered. Therefore, the content of Na 2 O is preferably 0 to 20% by weight.
Ｌｉ2Ｏはイオン交換処理において主としてナトリウムイオンと置換されることによってガラスを化学強化する成分であり、Ｎａ2Ｏよりもイオン交換速度が大きいため、短時間で深い圧縮応力層を形成するために用いられる。Ｌｉ2Ｏの含量が１５重量％を超えると耐失透性と化学耐久性が低下すると共に、圧縮応力層の最表面のナトリウムイオンの濃度が高くなり、Ｎａ溶出量が増加する。従って、Ｌｉ2Ｏの含有量は０〜１５重量％とすることが好ましい。 Li 2 O is a component that chemically strengthens glass by being mainly replaced with sodium ions in the ion exchange treatment, and has a higher ion exchange rate than Na 2 O, so that a deep compressive stress layer can be formed in a short time. Used. When the content of Li 2 O exceeds 15% by weight, devitrification resistance and chemical durability are lowered, the concentration of sodium ions on the outermost surface of the compressive stress layer is increased, and the amount of Na elution is increased. Therefore, the content of Li 2 O is preferably 0 to 15% by weight.
Ｌｉ2ＯとＮａ2Ｏの合計含有量が３重量％未満であると、イオン交換時の効率が低下し、充分な深さの圧縮応力層を形成することが難しくなる。一方、２０重量％を超えるとガラスの化学的耐久性、耐失透性がともに低下してしまう。従って、Ｌｉ2ＯとＮａ2Ｏの合計含有量は３〜２０重量％とすることが好ましい。 When the total content of Li 2 O and Na 2 O is less than 3% by weight, the efficiency at the time of ion exchange decreases, and it becomes difficult to form a compressive stress layer having a sufficient depth. On the other hand, when it exceeds 20% by weight, both the chemical durability and the devitrification resistance of the glass are lowered. Therefore, the total content of Li 2 O and Na 2 O is preferably 3 to 20% by weight.
ＺｒＯ2はイオン交換速度を向上させ、ガラスの化学的耐久性や硬さを向上させる成分であり、その含有量が９重量％を超えるとＺｒＯ2の溶解度が過飽和になり、原料が溶けずに沈殿状態となりやすい。従って、ＺｒＯ2の含有量は０．１〜９重量％であることが好ましい。 ZrO 2 is a component that improves the ion exchange rate and improves the chemical durability and hardness of the glass. If the content exceeds 9% by weight, the solubility of ZrO 2 becomes supersaturated and the raw material does not melt. It tends to be in a precipitated state. Therefore, the content of ZrO 2 is preferably 0.1 to 9% by weight.
また、このガラス基板は、溶融性の向上、耐失透性の向上、ガラス粘度の調整、歪み点の調整、熱膨張特性の調整、ヤング率の向上、清澄等の目的のため、Ｋ2Ｏ、ＭｇＯ、ＣａＯ、ＳｒＯ、ＢａＯ、ＺｎＯ、ＴｉＯ2、Ｂ2Ｏ3、Ｌａ2Ｏ3、Ｙ2Ｏ3、Ｐ2Ｏ5、ＳｎＯ2、Ｓｂ2Ｏ3、ＳＯ3等を含有することができる。上記成分のうち、ＭｇＯ、ＣａＯ、ＴｉＯ2、Ｙ2Ｏ3はヤング率を向上させる成分であり、適量含有させることによって曲げ変形に強いガラスが得られる。 In addition, this glass substrate is made of K 2 O for the purpose of improving meltability, improving devitrification resistance, adjusting glass viscosity, adjusting strain point, adjusting thermal expansion characteristics, improving Young's modulus, clarifying, etc. , MgO, CaO, SrO, BaO , ZnO, may contain TiO 2, B 2 O 3, La 2 O 3, Y 2 O 3, P 2 O 5, SnO 2, Sb 2 O 3, SO 3 , etc. it can. Among the above components, MgO, CaO, TiO 2 , and Y 2 O 3 are components that improve the Young's modulus, and a glass that is resistant to bending deformation can be obtained by adding an appropriate amount.
従って、本発明で用いられるガラス基板としては、ＳiＯ2を４０〜７０重量％、Ａｌ2Ｏ3を０．１〜２０重量％、Ｌｉ2Ｏを０〜１５重量％、Ｎａ2Ｏを０〜２０重量％、Ｌｉ2ＯとＮａ2Ｏの合計含有量が３〜２０重量％、ＺｒＯ2を０．１〜９重量％を含むガラスで形成されていることが望ましい。 Therefore, the glass substrate used in the present invention, the S i O 2 40 to 70 wt%, the Al 2 O 3 0.1 to 20 wt%, the Li 2 O 0 to 15 wt%, a Na 2 O It is desirable to be formed of glass containing 0 to 20% by weight, a total content of Li 2 O and Na 2 O of 3 to 20% by weight, and ZrO 2 of 0.1 to 9% by weight.
また、ＳｉＯ2を４５〜６５重量％、Ａｌ2Ｏ3を１〜２０重量％、Ｌｉ2Ｏを３〜１０重量％、Ｎａ2Ｏを３〜１５重量％、ＺｒＯ2を３〜８重量％、Ｓｂ2Ｏ3を０〜１重量％含むガラスで形成されていることがより好ましい。上記の望ましい組成及びより好ましい組成において、上記成分の合計含有量が８０重量％以上であることが好ましく、９０重量％以上であることがより好ましく、９５重量％以上であることがさらに好ましい。 Further, the SiO 2 45 to 65 wt%, the Al 2 O 3 1 to 20 wt%, the Li 2 O 3 to 10 wt%, 3-15 wt% of Na 2 O, the ZrO 2 3 to 8 wt% More preferably, it is made of glass containing 0 to 1% by weight of Sb 2 O 3 . In the desirable composition and the more preferable composition, the total content of the components is preferably 80% by weight or more, more preferably 90% by weight or more, and further preferably 95% by weight or more.
化学処理が施されるガラス基板として、上記組成のものが用いられる場合、化学強化処理を行うための処理塩としては、ナトリウムイオン及びカリウムイオンの少なくともいずれか一方を含む処理塩、例えば、ＮａＮＯ3、ＫＮＯ3又はこれらの混合物等を用いることができる。この場合、上記処理塩を３５０〜５５０℃程度に加熱して溶融塩とし、ガラス基板をこの溶融塩中に３０分〜６時間程度浸漬することによりイオン交換を行うことができる。これによって、ガラス基板に透明な圧縮応力層を形成することができる。 When the glass substrate subjected to the chemical treatment is used with the above composition, the treatment salt for performing the chemical strengthening treatment is a treatment salt containing at least one of sodium ions and potassium ions, for example, NaNO 3. , KNO 3 or a mixture thereof can be used. In this case, ion exchange can be performed by heating the treated salt to about 350 to 550 ° C. to form a molten salt and immersing the glass substrate in the molten salt for about 30 minutes to 6 hours. As a result, a transparent compressive stress layer can be formed on the glass substrate.
ガラス基板に上記の化学強化処理を施すことにより、ガラス基板中のアルカリ金属イオンの移動が抑制され、ガラス基板からのアルカリ金属の溶出量が低減される。従って、化学強化処理により液晶素子のアルカリ金属汚染を防止することも可能になる。ガラス基板からのアルカリ金属の溶出量を更に低減するためには、化学強化処理後に、ガラス基板を水又は酸水溶液で洗浄したり、ガラス基板を１２０℃以上好ましくは１５０℃以上に加熱してガラス基板表面のヒドロニウムイオンを除去したり、或いは、ガラス基板の表面にＳｉＯ2をコーティングするようにしてもよい。 By subjecting the glass substrate to the above chemical strengthening treatment, movement of alkali metal ions in the glass substrate is suppressed, and the amount of alkali metal eluted from the glass substrate is reduced. Therefore, alkali metal contamination of the liquid crystal element can be prevented by the chemical strengthening treatment. In order to further reduce the elution amount of alkali metal from the glass substrate, the glass substrate is washed with water or an aqueous acid solution after the chemical strengthening treatment, or the glass substrate is heated to 120 ° C. or higher, preferably 150 ° C. or higher. Hydronium ions on the surface of the substrate may be removed, or the surface of the glass substrate may be coated with SiO 2 .
また、ガラス基板に化学強化処理を施すことによって、ガラス基板の加熱、冷却に伴う寸法変化を抑制することもできる。これによって、液晶ディスプレイの製造工程における温度変化によってガラス基板の寸法が変化しにくくなる。従って、ガラス基板に薄膜や配線を重ねていく液晶ディスプレイの製造工程において構成部品の位置ずれが少なくなり、高精度の液晶ディスプレイを製造することが可能になる。 Moreover, the dimensional change accompanying a heating and cooling of a glass substrate can also be suppressed by performing a chemical strengthening process to a glass substrate. Thereby, the dimension of a glass substrate becomes difficult to change with the temperature change in the manufacturing process of a liquid crystal display. Accordingly, the positional displacement of the component parts is reduced in the manufacturing process of the liquid crystal display in which the thin film and the wiring are stacked on the glass substrate, and it becomes possible to manufacture a highly accurate liquid crystal display.
化学強化処理が施されたガラス基板に微小な傷（マイクロクラック）といったクラックソースがあると、このクラックソースが成長してガラスの破壊を発生させる原因となる。クラックソースは、化学強化された主表面に存在する場合よりも端面に存在する場合のほうが基板強度に与える影響が大きい。従って、強化処理が施される前のガラス基板又は強化処理が施されたガラス基板のクラックソースを除去することによって強度を向上させることができる。特に、ガラス基板端面のクラックソースを除去することが望ましい。 If there is a crack source such as a fine scratch (micro crack) on the glass substrate subjected to the chemical strengthening treatment, the crack source grows and causes the glass to break. The crack source has a greater influence on the substrate strength when it is present at the end face than when it is present at the chemically strengthened main surface. Therefore, the strength can be improved by removing the crack source of the glass substrate before being subjected to the tempering treatment or the glass substrate subjected to the tempering treatment. In particular, it is desirable to remove the crack source on the end face of the glass substrate.
クラックソースの除去方法には、エッチングによる方法、加熱軟化による方法等がある。エッチングによる方法では、ガラス基板を酸を含むエッチング液に浸漬し、マイクロクラックを除去し、クラックの先端を鈍化させることにより、基板強度を向上させる。このエッチング液としては、フッ酸を含有するもの、例えば、フッ酸と硫酸、塩酸、硝酸などとの混酸を用いることが好ましい。このような混酸、特にフッ酸を含む混酸を用いることによりガラス基板表面にエッチングによる副生成物が堆積せず、滑らかな面を形成することが可能になる。 The crack source removal method includes a method using etching, a method using heat softening, and the like. In the etching method, the substrate strength is improved by immersing the glass substrate in an etching solution containing an acid, removing the microcracks, and blunting the tips of the cracks. As this etching solution, it is preferable to use one containing hydrofluoric acid, for example, a mixed acid of hydrofluoric acid and sulfuric acid, hydrochloric acid, nitric acid or the like. By using such a mixed acid, particularly a mixed acid containing hydrofluoric acid, no by-product due to etching is deposited on the glass substrate surface, and a smooth surface can be formed.
このようなエッチング処理は、化学強化前のガラス基板に施すこともできるが、化学強化後に行うことにより圧縮応力層を緩和させることなくガラス基板表面のアルカリ金属を除去することができるので、化学強化後に施すことが望ましい。 Such etching treatment can be applied to the glass substrate before chemical strengthening, but it can be removed after the chemical strengthening because the alkali metal on the surface of the glass substrate can be removed without relaxing the compressive stress layer. It is desirable to apply it later.
加熱軟化による方法は、ガラスの端部をバーナーなどで加熱し、軟化させる。これによってマイクロクラックが塞がれ、端面が非接触の新たな非機械加工面になる。軟化によってガラス面の形状が変化した場合は、ガラス面のみを研磨することによってガラスの平坦性を確保することができる。加熱軟化による方法はガラスを軟化点以上に加熱しなければならないため、化学強化前に行なう必要がある。 In the method by heat softening, the edge of the glass is heated with a burner or the like to be softened. This closes the microcrack and creates a new non-machined surface with non-contacting end faces. When the shape of the glass surface changes due to softening, the flatness of the glass can be ensured by polishing only the glass surface. The method by heat softening must be performed before chemical strengthening because the glass must be heated above the softening point.
上述した化学強化処理が施されたガラス基板を切断すると、切断した端面は圧縮応力層のない未強化ガラスとなり、強度が極端に低下してしまう。本発明者は、化学強化処理により、曲げ強度が４００ＭＰａとなったガラス基板を切断すると、曲げ強度が約１００ＭＰａに低下することを確認した。従って、本発明のガラス基板は、予め使用時の寸法に加工されたガラス基板に強化処理を施して形成されることが好ましい。 When the glass substrate subjected to the above-described chemical strengthening treatment is cut, the cut end surface becomes unstrengthened glass without a compressive stress layer, and the strength is extremely reduced. The inventor has confirmed that the bending strength is reduced to about 100 MPa when the glass substrate having a bending strength of 400 MPa is cut by the chemical strengthening treatment. Therefore, it is preferable that the glass substrate of the present invention is formed by subjecting a glass substrate that has been processed in advance to a size during use to a strengthening treatment.
本発明のディスプレイ用ガラス基板は、圧縮応力層の厚さを越えない範囲で研磨を行なうことができる。本発明のガラス基板は、例えば、ＳＴＮ液晶ディスプレイ、ＴＦＴ液晶ディスプレイ、ＤＳＴＮ液晶ディスプレイ等の液晶ディスプレイや有機ＥＬディスプレイ、電界放出型ディスプレイ等に用いることができる。 The display glass substrate of the present invention can be polished within a range not exceeding the thickness of the compressive stress layer. The glass substrate of the present invention can be used for liquid crystal displays such as STN liquid crystal displays, TFT liquid crystal displays, and DSTN liquid crystal displays, organic EL displays, field emission displays, and the like.
特に、厚さを０．７ｍｍ以下としても、十分な強度を有しているので、モバイル型パーソナルコンピュータ、携帯電話、小型液晶テレビの表示装置といった携帯型ディスプレイに用いることができる。本発明のガラス基板は、厚さを薄く形成することにより、反射型液晶ディスプレイ、透過型液晶ディスプレイ、半透過型液晶ディスプレイなどの液晶ディスプレイ等に用いることができる。 In particular, even when the thickness is 0.7 mm or less, it has sufficient strength and can be used for portable displays such as mobile personal computers, mobile phones, and small liquid crystal television display devices. The glass substrate of the present invention can be used for a liquid crystal display such as a reflective liquid crystal display, a transmissive liquid crystal display, and a transflective liquid crystal display by forming a thin thickness.
以下、実施例により本発明をさらに説明する。
（実施例１〜３、５〜７、参考例４）表１の組成のガラス原料を白金坩堝で１４００〜１５００℃に加熱、溶融して、清澄を行なった後、鋳型に流し込んでガラスを調製した。ガラスが固化した後、ガラスをガラスの徐冷点付近に加熱された電気炉に移し、室温まで除冷してガラスブロックを得た。このガラスブロックから、厚さ０．４ｍｍ、３５×３５ｍｍの両面が研磨されたガラス基板を製造した。
Hereinafter, the present invention will be further described by examples.
(Examples 1-3, 5-7, Reference Example 4) Glass raw materials having the compositions shown in Table 1 were heated and melted at 1400-1500 ° C. in a platinum crucible, clarified, and then poured into a mold to prepare glass. did. After the glass solidified, the glass was transferred to an electric furnace heated near the annealing point of the glass, and cooled to room temperature to obtain a glass block. From this glass block, a glass substrate having a thickness of 0.4 mm and 35 × 35 mm polished on both sides was produced.
このガラス基板を所定温度に保持した溶融塩中に所定時間浸漬して化学強化処理を行い、両面に深さ５０μｍ以上の圧縮応力層を有する強化ガラス基板を得た。そして、得られた強化ガラス基板の未加傷曲げ強度及び加傷曲げ強度を測定した。未加傷曲げ強度はＪＩＳ−Ｒ１６０１の３点曲げ試験に準じて測定した。 This glass substrate was immersed in a molten salt maintained at a predetermined temperature for a predetermined time and subjected to a chemical strengthening treatment to obtain a strengthened glass substrate having a compressive stress layer having a depth of 50 μm or more on both sides. And the undamaged bending strength and wound bending strength of the obtained tempered glass substrate were measured. Unscratched bending strength was measured according to the three-point bending test of JIS-R1601.
加傷曲げ強度は♯１５０のサンドペーパーで強化ガラス基板の片面に均一に傷を付け、その面に引っ張り応力が働くようにして測定した。以上の結果、未加傷強度４００ＭＰａ以上、加傷曲げ強度２５０ＭＰａ以上の透明強化ガラス基板が得られた。 The scratch bending strength was measured by uniformly scratching one side of the tempered glass substrate with # 150 sandpaper and applying a tensile stress to the surface. As a result, a transparent tempered glass substrate having an unscratched strength of 400 MPa or more and a scratch bending strength of 250 MPa or more was obtained.
（実施例８）実施例１で得られた強化ガラス基板を５％希フッ酸と３０％硫酸の混合水溶液に室温で５分間浸漬してエッチング処理を行った。このようなエッチング処理が施された強化ガラス基板の未加傷曲げ強度は５５０ＭＰａであり、エッチングが施されていない実施例１の値と比較し、１０％程度向上させることができた。 (Example 8) The tempered glass substrate obtained in Example 1 was etched by being immersed in a mixed aqueous solution of 5% dilute hydrofluoric acid and 30% sulfuric acid at room temperature for 5 minutes. The undamaged bending strength of the tempered glass substrate subjected to such an etching treatment was 550 MPa, which was improved by about 10% compared to the value of Example 1 where the etching was not performed.
（実施例９）実施例８で得られた強化ガラス基板（厚さ０．４ｍｍ、３５×３５ｍｍ）を用いて１．８インチの半透過型ＳＴＮ液晶ディスプレイを作製した。このディスプレイでは厚さ１ｍｍの強化ガラス基板を用いた液晶ディスプレイに比べた場合輝度を２０％程度向上させることができた。また、基板の厚みを０．７ｍｍとした場合には、従来品より輝度を１０％程度向上させることができた。 Example 9 A 1.8-inch transflective STN liquid crystal display was produced using the tempered glass substrate (thickness 0.4 mm, 35 × 35 mm) obtained in Example 8. In this display, the luminance can be improved by about 20% when compared with a liquid crystal display using a tempered glass substrate having a thickness of 1 mm. Moreover, when the thickness of the substrate was 0.7 mm, the luminance could be improved by about 10% compared to the conventional product.
この強化ガラス基板は十分な加傷曲げ強度を有しているので、ディスプレイ製造過程で基板が損傷する可能性を低減し、しかも使用の際に予想される加傷に対して充分な耐久性を有するディスプレイを提供することができた。 Since this tempered glass substrate has sufficient scratch bending strength, the possibility of damaging the substrate during the display manufacturing process is reduced, and sufficient durability against damage expected during use is provided. It was possible to provide a display having.
（比較例１〜３）表２の組成のガラス原料を用い実施例１〜７と同一の方法でガラス基板を製造した。このガラス基板を所定温度に保持した処理塩中に所定時間浸漬して化学強化処理を行い、両主表面に圧縮応力層を有する強化ガラス基板を得た。そして、実施例１〜７と同様の方法で強化ガラス基板の未加傷曲げ強度及び加傷曲げ強度を測定した。 Comparative Examples 1 to 3 Glass substrates were produced in the same manner as in Examples 1 to 7, using glass raw materials having the compositions shown in Table 2. This glass substrate was immersed in a treatment salt maintained at a predetermined temperature for a predetermined time to perform a chemical strengthening treatment to obtain a strengthened glass substrate having compressive stress layers on both main surfaces. And the undamaged bending strength and bruised bending strength of the tempered glass substrate were measured by the same method as Examples 1-7.
その結果、未加傷曲げ強度は１００〜４５０ＭＰａと充分なものもあったが、加傷曲げ強度は７０ＭＰａ以下であり、これでは基板の厚さを薄くして軽量化した場合、使用時に傷が付くと割れやすく、実用に耐え得るものではなかった。 As a result, there were some unscratched bending strengths of 100 to 450 MPa, but the scratching bending strength was 70 MPa or less. In this case, when the thickness of the substrate was reduced and the weight was reduced, there was no damage during use. When attached, it was easy to break and could not withstand practical use.
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