WO2013018774A1 - 化学強化ガラスの衝撃試験方法、化学強化ガラスの割れ再現方法及び化学強化ガラスの製造方法 - Google Patents
化学強化ガラスの衝撃試験方法、化学強化ガラスの割れ再現方法及び化学強化ガラスの製造方法 Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/30—Investigating strength properties of solid materials by application of mechanical stress by applying a single impulsive force, e.g. by falling weight
- G01N3/303—Investigating strength properties of solid materials by application of mechanical stress by applying a single impulsive force, e.g. by falling weight generated only by free-falling weight
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M7/00—Vibration-testing of structures; Shock-testing of structures
- G01M7/08—Shock-testing
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- the present invention relates to an impact test method for chemically strengthened glass in which a compressive stress layer is formed by chemical strengthening, a crack reproduction method for chemically strengthened glass, and a method for producing chemically strengthened glass.
- the conventional cover glass chemically strengthens the glass plate to form a compressive stress layer on the surface to improve the scratch resistance of the cover glass (for example, Patent Document 1).
- an object of the present invention is to provide an impact test method for chemically strengthened glass that can reproduce slow crack cracks in chemically strengthened glass, a method for reproducing cracks in chemically strengthened glass, and a method for producing chemically strengthened glass. .
- the inventors of the present invention have clarified the mechanism of slow crack cracking in researching and researching slow crack cracking, and have reached the present invention.
- the present invention provides the following aspects.
- (1) A method for impact test of chemically strengthened glass having a compressive stress layer formed on a surface thereof, In the state where the chemically strengthened glass is disposed on a base, and one surface of the chemically strengthened glass is brought into contact with a rubbing surface of a sandpaper containing an abrasive having a size larger than the depth of the compressive stress layer, Impact test method for chemically strengthened glass dropped from above.
- the chemical tempered glass has a tapered tip portion having a length equal to or greater than the depth of the compressive stress layer and collides with an impact object having a higher hardness than the chemical tempered glass on one surface of the chemical tempered glass.
- the method for reproducing cracks in the chemically strengthened glass according to (4) (9) The method for reproducing cracks in chemically strengthened glass according to (8), wherein a scattering prevention film is stretched on the other surface of the chemically strengthened glass that does not collide with the impact object. (10) A method for producing chemically strengthened glass having a compressive stress layer formed on a surface thereof, While changing the falling ball height of the sphere, the threshold value is determined by the impact test method for chemically strengthened glass according to any one of (1) to (3), A method for producing chemically tempered glass, wherein a sampling inspection for judging the quality of the chemically tempered glass is performed based on the threshold value.
- FIG. 1 is a schematic view showing a situation in which a slow crack occurs in a cover glass when a flat panel display device falls.
- FIG. 2A is a schematic diagram showing a starting point of breakage when a slow crack occurs
- FIG. 2B is a schematic view showing a crack generated from the starting point of FIG. 2A.
- FIG. 3A is a diagram showing a photograph of a flat panel display device in which a slow crack is generated
- FIG. 3B is a diagram showing an enlarged photograph of the fracture starting point as viewed from above
- FIG. It is a figure which shows the photograph which looked at the starting point from the side.
- FIG. 4 is a diagram schematically showing a fracture surface of FIG. FIG.
- FIG. 5 is a view showing a photograph of the break starting point of the cover glass in which non-slow crack cracking is seen from the side.
- FIG. 6 is a diagram schematically showing the fracture surface of FIG.
- FIG. 7 is a schematic diagram of the slow crack crack reproduction method of the first embodiment.
- FIG. 8A is a schematic diagram showing a fracture starting point when a chemically tempered glass crack occurs in the slow crack crack reproducing method of FIG. 7, and
- FIG. 8B is a plan view of the fracture starting point of FIG. 8A. It is a schematic diagram which shows the generated crack.
- FIG. 9 is a schematic diagram of a method for reproducing a slow crack crack according to a modification.
- FIG. 9 is a schematic diagram of a method for reproducing a slow crack crack according to a modification.
- FIG. 10 (a) is a schematic diagram showing the starting point of breakage when chemically tempered glass cracking occurs in the method for reproducing slow cracking in FIG. 9, and FIG. 10 (b) is the starting point of breaking in FIG. 10 (a). It is a schematic diagram which shows the generated crack.
- FIG. 11 is a schematic diagram of a slow crack crack reproduction method according to the second embodiment. 12A is an enlarged photograph of P30 sandpaper, FIG. 12B is an enlarged photograph of asphalt concrete, and FIG. 12C is the angle of the P30 sandpaper tip. It is a graph which shows distribution and angle distribution of the front-end
- FIGS. 13 (a) to 13 (c) are photographs showing chemically tempered glass broken in Examples 1 to 3. FIG. FIG. FIG.
- FIG. 14 is a view showing a photograph of the fracture starting point in Example 1 viewed from the side.
- FIGS. 15A to 15E are photographs showing chemically tempered glass cracked in Examples 4 to 7 and Comparative Example 1.
- FIG. FIG. 16 is a view showing a photograph of the fracture starting point in Example 4 as viewed from the side.
- FIG. 17 is a photograph of broken chemically strengthened glass in a method for reproducing slow cracking using P30 (D 3 : 710 ⁇ m) sandpaper.
- FIG. 18 is a photograph of a chemically strengthened glass that was cracked in a method for reproducing slow cracking using a P100 (D 3 : 180 ⁇ m) sandpaper.
- FIG. 1 is a schematic diagram showing a situation where a slow crack crack is generated in the cover glass when the flat panel display device is dropped
- FIG. 2A is a schematic diagram showing a fracture starting point when the slow crack crack is generated
- FIG. 3B is a schematic diagram showing a crack generated from the fracture starting point in FIG. 2A
- FIG. 3A is a diagram showing a photograph of a flat panel display device in which a slow crack crack has occurred
- FIG. 3C is a diagram showing an enlarged photograph of the starting point seen from above
- FIG. 3C is a diagram showing a photograph of the fracture starting point seen from the side.
- the flat panel display device is provided with a substantially rectangular frame so as to surround the image display unit, and a cover glass is supported on the frame.
- a cover glass is supported on the frame.
- FIG. 1 when the flat panel display device falls on the ground (asphalt / concrete) and the cover glass 2 faces downward, it contacts the sand 5 etc. on the pebbles 4 in the asphalt / concrete 3; A compressive stress acts on the fracture starting point O, and a tensile stress acts around it (FIG. 2 (a)). Subsequently, a tensile stress acts on the fracture starting point O, the crack C extends, and the cover glass 2 is broken (FIG. 2B). Note that the breakage starting point may occur in the center portion of the cover glass, but often occurs in a part of the region supported by the frame because the bending of the cover glass is restrained by the frame.
- the crack of the cover glass 2 at this time has a fracture starting point that is deeper than the depth of the compressive stress layer, as is apparent from the fracture surface of FIG. In FIG. 3 (a) and (b), one crack extends from the fracture starting point, and the cover glass is broken into two.
- a mirror with a smooth mirror radius is seen around the fracture starting point deeper than the depth of the compressive stress layer. .
- FIG. 4 is a diagram schematically showing the fracture surface of FIG.
- the fracture surface reflects factors such as the process of destruction, that is, the origin of the destruction, the direction of the destruction, whether the destruction progressed slowly or rapidly.
- the mirror surface with a long mirror radius means that the fracture progressed due to a small stress. It means that it grew at a much slower rate. Therefore, according to the fractured surface of FIG. 3 (c), it can be seen that after the starting point deeper than the depth of the compressive stress layer was formed on the cover glass, cracks grew slowly and the fracture proceeded with a small stress.
- a cover glass that has been cracked by such slow cracking has several to several tens of pieces. Typically, it is 2 to 20 pieces, and an example in which one crack extends from the fracture starting point shown in FIGS. 3 (a) and 3 (b) and the cover glass breaks into two is a symbol of slow crack cracking. Example.
- FIG. 5 is a view showing a photograph of a cover glass breakage starting point caused by non-slow crack cracking as viewed from the side
- FIG. 6 is a view schematically showing a broken surface of FIG.
- the cover glass becomes a plurality (20 or more) of glass pieces due to a plurality of cracks extending in the shape of a spider web, as shown in FIG. This is also called spider cracking.)
- the slow crack crack and the non-slow crack crack are broken in completely different modes.
- the slow crack crack is a crack generated by forming a fracture starting point deeper than the depth of the compressive stress layer.
- the crack fragment is 2 pieces to 20 pieces.
- the non-slow cracking generated from the starting point in the compressive stress layer is a completely different mode because it becomes a shattered glass piece.
- the sandpaper in the present invention is not limited to abrasive paper (sandpaper, JIS R6252: 2006), and includes a substrate coated with an abrasive with an adhesive, or equivalent, such as abrasive cloth (JIS R6251: 2006). ), Water resistant abrasive paper (JIS R6253: 2006) and the like.
- the material and weight of the sphere 13 can be changed according to the purpose, but typically, a stainless steel ball of 4 to 150 g made of SUS is used.
- FIG. 9 shows a modification of the first embodiment.
- a sandpaper 12 containing an abrasive having a size larger than the depth of the compressive stress layer is disposed below the chemically strengthened glass 10, and the lower surface 10b of the chemically strengthened glass 10 is sand.
- the sphere 13 is dropped onto the upper surface 10 a of the chemically strengthened glass 10.
- the fracture start point O is deeper than the compressive stress layer on the lower surface 10 b side due to the abrasive contained in the sandpaper 12. Will occur.
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Abstract
Description
(1)表面に圧縮応力層が形成された化学強化ガラスの衝撃試験方法であって、
前記化学強化ガラスを基台上に配置し、前記圧縮応力層の深さ以上の大きさの研磨材を含むサンドペーパーの擦り面に前記化学強化ガラスの一面を接触させた状態で、衝撃物を上方から落下させる化学強化ガラスの衝撃試験方法。
(2)前記サンドペーパーは、前記化学強化ガラスの上方に配置する(1)に記載の化学強化ガラスの衝撃試験方法。
(3)前記サンドペーパーの擦り面に接触しない前記化学強化ガラスの他面に、飛散防止フィルムを張る(1)又は(2)に記載の化学強化ガラスの衝撃試験方法。
(4)表面に圧縮応力層が形成された化学強化ガラスの割れ再現方法であって、
前記化学強化ガラスに、衝撃を与えて前記圧縮応力層より深い傷をつける化学強化ガラスの割れ再現方法。
(5)前記化学強化ガラスを基台上に配置し、前記圧縮応力層の深さ以上の大きさの研磨材を含むサンドペーパーの擦り面に化学強化ガラスの一面を接触させた状態で、衝撃物を上方から落下させる(4)に記載の化学強化ガラスの割れ再現方法。
(6)前記サンドペーパーは、前記化学強化ガラスの上方に配置する(5)に記載の化学強化ガラスの割れ再現方法。
(7)前記サンドペーパーの擦り面に接触しない前記化学強化ガラスの他面に、飛散防止フィルムを張る(5)又は(6)に記載の化学強化ガラスの割れ再現方法。
(8)前記化学強化ガラスに対し、前記圧縮応力層の深さ以上の長さの先細状の先端部を有し、前記化学強化ガラスより硬度の高い衝撃物を前記化学強化ガラスの一面に衝突させる(4)に記載の化学強化ガラスの割れ再現方法。
(9)前記衝撃物が衝突しない前記化学強化ガラスの他面に、飛散防止フィルムを張る(8)に記載の化学強化ガラスの割れ再現方法。
(10)表面に圧縮応力層が形成された化学強化ガラスの製造方法であって、
前記球体の落球高さを変えながら(1)~(3)のいずれかに記載の化学強化ガラスの衝撃試験方法により閾値を決定し、
該閾値を基準に前記化学強化ガラスの品質を判定する抜き取り検査を行う化学強化ガラスの製造方法。
図1はフラットパネルディスプレイ装置が落下した際にカバーガラスにスロークラック割れが発生する状況を示す模式図、図2(a)はスロークラック割れが発生するときの破壊起点を示す模式図、図2(b)は図2(a)の破壊起点から発生したクラックを示す模式図、図3(a)はスロークラック割れが発生したフラットパネルディスプレイ装置の写真を示す図、図3(b)は破壊起点を上方から見た拡大写真を示す図、図3(c)は破壊起点を側方から見た写真を示す図である。
第1実施形態のスロークラック割れの再現方法は、図7に示すように、表面に圧縮応力層が形成された化学強化ガラス10を基台11上に配置し、圧縮応力層の深さ以上の大きさの研磨材を含むサンドペーパー12の擦り面12aに化学強化ガラス10を接触させ、鉄球等の球体13を上方から落下させるものである。このとき、サンドペーパー12は、好ましくは化学強化ガラス10の上方に配置され、化学強化ガラス10の上面10aがサンドペーパー12の擦り面12aと接触しており、球体13がサンドペーパー12の擦り面12aとは反対側の面12bに落下する。
化学強化ガラスは3枚に割れているが、図14は図3(c)と同様の破断面を示しており、スロークラック割れと同じメカニズムで割れが発生していることが分かる。
本変形では、図9に示すように、圧縮応力層の深さ以上の大きさの研磨材を含むサンドペーパー12が、化学強化ガラス10の下方に配置され、化学強化ガラス10の下面10bがサンドペーパー12の擦り面12aと接触しており、球体13を化学強化ガラス10の上面10aに落下させるものである。
化学強化ガラスは6枚に割れているが、図16は図3(c)と同様の破断面を示しており、スロークラック割れと同じメカニズムで割れが発生していることが分かる。
第2実施形態のスロークラック割れの再現方法は、図11に示すように、表面に圧縮応力層が形成された化学強化ガラス10に、圧縮応力層の深さ以上の長さの先細状の先端部21を有し、化学強化ガラス10より硬度の高い衝撃物22を化学強化ガラス10に衝突させるものである。
(i)モル%で表示した組成で、SiO2を50~80%、Al2O3を2~25%、Li2Oを0~10%、Na2Oを0~18%、K2Oを0~10%、MgOを0~15%、CaOを0~5%およびZrO2を0~5%を含むガラス。ここで、例えば「K2Oを0~10%含む」とはK2Oは必須ではないが10%までの範囲で、かつ、本発明の目的を損なわない範囲で含んでもよい、の意である(以下、同様)。
(ii)モル%で表示した組成が、SiO2を50~74%、Al2O3を1~10%、Na2Oを6~14%、K2Oを3~11%、MgOを2~15%、CaOを0~6%およびZrO2を0~5%含有し、SiO2およびAl2O3の含有量の合計が75%以下、Na2OおよびK2Oの含有量の合計が12~25%、MgOおよびCaOの含有量の合計が7~15%であるガラス。
(iii)モル%で表示した組成が、SiO2を68~80%、Al2O3を4~10%、Na2Oを5~15%、K2Oを0~1%、MgOを4~15%およびZrO2を0~1%含有するガラス。
(iv)モル%で表示した組成が、SiO2を67~75%、Al2O3を0~4%、Na2Oを7~15%、K2Oを1~9%、MgOを6~14%およびZrO2を0~1.5%含有し、SiO2およびAl2O3の含有量の合計が71~75%、Na2OおよびK2Oの含有量の合計が12~20%であり、CaOを含有する場合その含有量が1%未満であるガラス。
厚さ0.7mm、サイズ:50mm×50mmの化学強化用ガラスをフロート法で製造し、435℃の硝酸カリウム(KNO3)溶融塩に4時間浸漬させることで化学強化を行った。化学強化後の表面圧縮応力は約800MPaであり、圧縮応力層の深さは約45μmであった。化学強化された化学強化ガラスは、表面に傷がつかないように、また、表面が他のものに接触しないようにカセットにて搬送し、破壊起点となる面とは反対側の面に飛散防止フィルムを張った。
図13(a)~(c)から実施例1~3のいずれにおいても、ガラス片が20枚以下であった。また、図14に示す破断面を観察すると、圧縮応力層の深さより深い傷を破壊起点として、破壊起点の回りには鏡のように滑らかな鏡面半径の長い鏡面が見られた。これにより、実施例1~3で、スロークラック割れを再現できた。また、実施例1~3を比べると、球体の落球高さが低くなるほど、割れたガラス片の数が減少する結果となった。
図15(a)~(d)から実施例4~7のいずれにおいても、ガラス片が20枚以下であった。また、図16に示す破断面を観察すると、圧縮応力層の深さより深い破壊起点が形成され、破壊起点の回りには、滑らかな破断面が存在し、さらにその回りに鏡のように滑らかな鏡面半径の長い鏡面が見られた。これにより、実施例4~7で、スロークラック割れを再現できた。また、実施例4と実施例5、実施例6と実施例7をそれぞれ比べると、球体の落球高さが低くなるほど、割れたガラス片の数が減少する結果となった。さらに、実施例4と実施例6、実施例5と実施例7をそれぞれ比べると、メッシュが小さくなるほど、即ち粒径が大きくなるほど、割れたガラス片の数が減少する結果となった。
3 アスファルト・コンクリート
4 小石
5 砂
10 化学強化ガラス
10a 上面
11 基台
12 サンドペーパー
12a 擦り面
13 球体
O 破壊起点
C クラック
Claims (10)
- 表面に圧縮応力層が形成された化学強化ガラスの衝撃試験方法であって、
前記化学強化ガラスを基台上に配置し、前記圧縮応力層の深さ以上の大きさの研磨材を含むサンドペーパーの擦り面に前記化学強化ガラスの一面を接触させた状態で、衝撃物を上方から落下させる化学強化ガラスの衝撃試験方法。 - 前記サンドペーパーは、前記化学強化ガラスの上方に配置する請求項1に記載の化学強化ガラスの衝撃試験方法。
- 前記サンドペーパーの擦り面に接触しない前記化学強化ガラスの他面に、飛散防止フィルムを張る請求項1又は2に記載の化学強化ガラスの衝撃試験方法。
- 表面に圧縮応力層が形成された化学強化ガラスの割れ再現方法であって、
前記化学強化ガラスに、衝撃を与えて前記圧縮応力層より深い傷をつける化学強化ガラスの割れ再現方法。 - 前記化学強化ガラスを基台上に配置し、前記圧縮応力層の深さ以上の大きさの研磨材を含むサンドペーパーの擦り面に化学強化ガラスの一面を接触させた状態で、衝撃物を上方から落下させる請求項4に記載の化学強化ガラスの割れ再現方法。
- 前記サンドペーパーは、前記化学強化ガラスの上方に配置する請求項5に記載の化学強化ガラスの割れ再現方法。
- 前記サンドペーパーの擦り面に接触しない前記化学強化ガラスの他面に、飛散防止フィルムを張る請求項5又は6に記載の化学強化ガラスの割れ再現方法。
- 前記化学強化ガラスに対し、前記圧縮応力層の深さ以上の長さの先細状の先端部を有し、前記化学強化ガラスより硬度の高い衝撃物を前記化学強化ガラスの一面に衝突させる請求項4に記載の化学強化ガラスの割れ再現方法。
- 前記衝撃物が衝突しない前記化学強化ガラスの他面に、飛散防止フィルムを張る請求項8に記載の化学強化ガラスの割れ再現方法。
- 表面に圧縮応力層が形成された化学強化ガラスの製造方法であって、
前記球体の落球高さを変えながら請求項1~3のいずれか1項に記載の化学強化ガラスの衝撃試験方法により閾値を決定し、
該閾値を基準に前記化学強化ガラスの品質を判定する抜き取り検査を行う化学強化ガラスの製造方法。
Priority Applications (4)
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JP2013526920A JP5994780B2 (ja) | 2011-08-04 | 2012-07-30 | 化学強化ガラスの衝撃試験方法 |
KR1020147002434A KR101935076B1 (ko) | 2011-08-04 | 2012-07-30 | 화학 강화 유리의 충격 시험 방법, 화학 강화 유리의 깨짐 재현 방법 및 화학 강화 유리의 제조 방법 |
CN201280038675.4A CN103782152B (zh) | 2011-08-04 | 2012-07-30 | 化学强化玻璃的冲击试验方法、化学强化玻璃的裂纹再现方法及化学强化玻璃的制造方法 |
US14/172,061 US9470614B2 (en) | 2011-08-04 | 2014-02-04 | Method for impact-testing chemically strengthened glass, method for reproducing cracks in chemically strengthened glass, and method for manufacturing chemically strengthened glass |
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US14/172,061 Continuation US9470614B2 (en) | 2011-08-04 | 2014-02-04 | Method for impact-testing chemically strengthened glass, method for reproducing cracks in chemically strengthened glass, and method for manufacturing chemically strengthened glass |
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US11634359B2 (en) | 2014-02-24 | 2023-04-25 | Corning Incorporated | Strengthened glass with deep depth of compression |
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JPWO2013018774A1 (ja) | 2015-03-05 |
JP5994780B2 (ja) | 2016-09-21 |
KR20140056244A (ko) | 2014-05-09 |
US9470614B2 (en) | 2016-10-18 |
KR101935076B1 (ko) | 2019-01-03 |
CN103782152B (zh) | 2015-11-25 |
TW201314203A (zh) | 2013-04-01 |
CN103782152A (zh) | 2014-05-07 |
US20140150525A1 (en) | 2014-06-05 |
TWI580961B (zh) | 2017-05-01 |
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