JP2007238378A - Glass plate having high fracture toughness and method of manufacturing the same - Google Patents

Glass plate having high fracture toughness and method of manufacturing the same Download PDF

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Publication number
JP2007238378A
JP2007238378A JP2006063693A JP2006063693A JP2007238378A JP 2007238378 A JP2007238378 A JP 2007238378A JP 2006063693 A JP2006063693 A JP 2006063693A JP 2006063693 A JP2006063693 A JP 2006063693A JP 2007238378 A JP2007238378 A JP 2007238378A
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Japan
Prior art keywords
glass plate
fracture toughness
glass
ion implantation
ions
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JP2006063693A
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Japanese (ja)
Inventor
Takashi Iwano
Shuhei Tanaka
隆史 岩野
修平 田中
Original Assignee
Central Glass Co Ltd
Shuhei Tanaka
セントラル硝子株式会社
修平 田中
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Application filed by Central Glass Co Ltd, Shuhei Tanaka, セントラル硝子株式会社, 修平 田中 filed Critical Central Glass Co Ltd
Priority to JP2006063693A priority Critical patent/JP2007238378A/en
Publication of JP2007238378A publication Critical patent/JP2007238378A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0005Other surface treatment of glass not in the form of fibres or filaments by irradiation
    • C03C23/0055Other surface treatment of glass not in the form of fibres or filaments by irradiation by ion implantation

Abstract

<P>PROBLEM TO BE SOLVED: To provide a glass plate having strength and fracture toughness improved by forming a modified phase on the surface of the glass plate. <P>SOLUTION: Nitrogen ion or silicon ion is implanted into the surface of the glass plate in a depth of 10 nm to 10μm from the surface in the implantation amount of 1×10<SP>12</SP>-1×10<SP>18</SP>ions/cm<SP>2</SP>. The number of layers to be ion-implanted is one or more layers. The ion-implantation is carried out at 0.05-50 μA/cm<SP>2</SP>ion current and the thickness of the ion implanted layer is changed by continuously changing the acceleration voltage in the ion-implantation. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to the modification of the surface of a glass plate, and more particularly to a glass plate having high fracture toughness and a method for producing the same.

  In recent years, there has been a demand for weight reduction of a large area display device such as a flat panel type PDP and a liquid crystal display which are widely used, and a display device used for a mobile phone. The glass plate used is required to be thin.

  The strength and fracture toughness value of the glass plate are not sufficient, and it is strongly desired to improve the strength and fracture toughness with the reduction in thickness. In addition, the glass used for the glass plate has many limitations because it requires physical properties according to the purpose, and it is difficult to change the glass composition of the glass plate, and the strength and fracture toughness are changed by changing the glass composition. It is difficult to improve without

Patent Document 1 discloses a technique for modifying the surface of glass by an ion implantation method. This technique is a technique for suppressing elution of alkali components such as Na in glass, and no attempt has been made to improve mechanical properties.
JP-A-5-85777

  Provided is a glass plate having improved strength and fracture toughness by forming a modified phase on the surface of the glass plate.

The glass plate having high fracture toughness according to the present invention is a glass plate obtained by implanting ions on the surface, wherein the ions are nitrogen ions or silicon ions, and the ion implantation depth is in the range of 10 nm to 10 μm from the surface. The glass plate having high fracture toughness characterized by having an ion implantation amount of 1 × 10 12 ions / cm 2 to 1 × 10 18 ions / cm 2 .

  The glass plate having high fracture toughness according to the present invention is characterized in that in the glass plate having high fracture toughness, a plurality of ion implantation layers of two or more layers are formed. A glass substrate having high fracture toughness as described above.

Further, the method for producing a glass plate having high fracture toughness according to the present invention is the method for producing a glass plate having high fracture toughness, wherein ions are implanted in an injection current range of 0.05 μA / cm 2 to 50 μA / cm 2. It is the manufacturing method of the glass plate which has high fracture toughness characterized by doing.

  Further, the method for producing a glass plate having high fracture toughness according to the present invention is the method for producing a glass plate having high fracture toughness, wherein the acceleration voltage at the time of ion implantation is continuously changed to reduce the thickness of the ion implantation layer. It is a manufacturing method of a glass substrate having high fracture toughness characterized by changing.

  The glass plate having high fracture toughness and the manufacturing method thereof according to the present invention are a glass having high fracture toughness having high fracture toughness by improving fracture toughness by injecting ions into the glass plate and enhancing resistance to scratches and cracks. Allows you to provide a board.

  In the present invention, ions are implanted into the surface layer of a glass plate such as soda lime glass by an ion implantation method, the surface layer of the glass plate is modified, the hardness of the surface of the glass plate is reduced, and the fracture toughness is improved. It is.

  Here, the fracture toughness is a value (K1c) calculated by the following equation in the fracture toughness measurement method (IF method) of JIS1607.

K1c = 0.026 · E 1/2 · P 1/2 · a · C 3/2
Here, E: Young's modulus, P: indentation load, a: half of the average indentation diagonal length, C: half of the average crack length
FIG. 1 conceptually shows a manufacturing method for modifying a glass surface layer by ion implantation, in which an ion-implanted layer 2 is formed at a depth of several hundred nm on the surface layer of a glass plate 1.

  The on-implant layer 2 uses an ion implantation apparatus as shown in FIG. 2 and the ions generated in the ion source 3 are accelerated by the acceleration voltage in the high voltage unit 5, and the accelerated ions are transferred to the implantation chamber 8. It is injected and formed on the surface of a glass plate (not shown) to be set. Ions are preferably implanted into the glass plate 1 at a constant acceleration voltage and injection current. By controlling the amount of ions, a glass plate with improved fracture toughness can be obtained.

  The depth t from the glass plate surface of the on-implanted layer 2 can be changed by changing the acceleration voltage at the time of ion implantation. As shown in FIG. 1, the depth t of the ion-implanted layer 2 is preferably in the range of 10 nm to 10 μm at the center of the ion-implanted layer, and the ion-implanted layer is preferably formed at a position shallower than 500 nm. If the ion-implanted layer is too deep, the influence on the surface layer is reduced, and a sufficient effect of improving fracture toughness cannot be obtained.

  Further, the glass plate 1 for performing ion implantation is not particularly limited. For example, oxide glass (quartz glass, silicate glass, borosilicate glass, phosphate glass, aluminum silicate glass, etc.), halide glass, and the like. , Sulfide glass or chalcogenide glass. In particular, a glass plate containing a large amount of alkali is preferable as the glass used in the present invention because the implantation time such as ion implantation current and ion implantation amount can be shortened. In addition to the glass plate, various materials such as plastic and ceramics can be used.

  Further, the thickness of the ion implantation layer can be made thicker or thinner by performing implantation while changing the acceleration voltage. High destruction Further, it is also possible to form two or more ion-implanted layers by implanting ions in the same sample while changing the acceleration voltage. Changing the thickness of the ion-implanted layer and forming two or more ion-implanted layers are preferable because large fracture toughness can be obtained.

  The ions implanted in the ion implantation layer 2 are preferably ions having a relatively large ion radius, such as nitrogen (N) and (silicon) Si.

Moreover, it is desirable that the injection current at the time of ion implantation into the glass plate be in the range of 0.05 μA / cm 2 to 50 μA / cm 2 .

If the implantation current is smaller than 0.05 μA / cm 2 , the ion implantation time becomes long, which is not preferable. On the other hand, if the implantation current is larger than 50 μA / cm 2 , the glass structure is destroyed and the ion implantation effect cannot be obtained.

The amount of ions to be implanted into the glass plate is preferably 1E18ions / cm 2 from 1E12ions / cm 2 in an amount of ions per 1 cm 2. This is because the ion implantation amount needs to be an amount that does not destroy the structure inside the glass, and if the amount is too small, a large effect cannot be obtained.

  As shown in Example 1, the glass plate having high fracture toughness of the present invention is also a glass plate having high bending strength.

  Furthermore, the fracture toughness is improved by the ion implantation of the present invention to the glass with high strength such as glass having a high refractive index near the surface using an ultrashort pulse laser, air-cooled tempered glass, chemically tempered glass, etc. It is possible to increase the strength of the glass.

Nitrogen (N) ions are implanted into the surface of soda lime silicate glass (SiO 2 —Na 2 O—CaO) having an area of 40 mm × 4 mm and a thickness of 2 mm using an ion implantation apparatus as shown in FIG. A glass plate having fracture toughness was produced.

An ion acceleration voltage of 150 keV and an implantation current of 15 μA were used to form an N ion implantation layer centered on approximately 310 nm from the glass surface layer. The ion implantation amount was 2 × 10 16 ions / cm 2 .

A glass plate having high fracture toughness was produced in the same manner as in Example 1 except that the ion implantation amount was 1 × 10 16 ions / cm 2 .

A glass plate having high fracture toughness was produced in the same manner as in Example 1 except that the nitrogen ion implantation current was 30 μA and the ion implantation amount was 1 × 10 16 ions / cm 2 .

A glass plate having high fracture toughness was produced in the same manner as in Example 1 except that the ions to be implanted were silicon (Si) ions.
Comparative Example 1
The soda lime silicate glass (SiO 2 —Na 2 O—CaO) having an area of 40 mm × 4 mm and a thickness of 2 mm used in Examples 1 to 3 was used as a comparative example without ion implantation.

  Table 1 shows Vickers hardness, crack generation load, and fracture toughness measured in accordance with JIS 1607 for Examples 1 to 3 and Comparative Example 1. The crack generation load is a load when a crack is generated in the indentation when the Vickers hardness is measured. FIG. 3 shows an example in which no crack is generated in the indentation in the example, and FIG. 4 shows a state in which the crack is generated in the indentation of the comparative example.

  As shown in Table 1, in the examples, the Vickers hardness was smaller than that of the comparative example, the load causing cracks in the indentation was larger than that of the comparative example, and the glass was soft on the surface. Moreover, the value of fracture toughness was also better than that of the comparative example.

Moreover, the bending strength of Example 1 was about 230 MPa, and was higher than that of Comparative Example 1 of 150 MPa.
The crack generation load and fracture toughness value (K1c) of the glass plate having high fracture toughness of Example 4 were higher than those of Comparative Example 1, and the Vickers hardness was small.

  The high fracture toughness material of the present invention can be widely used as a glass with improved fracture toughness of glass for a wide range of uses such as glass plates used for display devices such as glass for PDP and glass for liquid crystal displays, glass for vehicles, and residential glass. .

It is sectional drawing which shows notionally the glass plate which has the high fracture toughness of this invention. It is the schematic of an ion implantation apparatus. FIG. 3 is a photomicrograph for a drawing in which cracks do not occur in the indentation of Example 1. FIG. The photomicrograph for the drawing substitute which the crack generate | occur | produced in the indentation of the comparative example 1.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Glass plate 2 Ion implantation layer 3 Ion source 4 of ion implantation apparatus 4 Shield cabinet 5 High voltage part 6 Accelerating tube 7 Beam line 8 Injection chamber 9 Clean unit 10 Glass 11 which formed the ion implantation layer 11 Vickers indentation impression 12 Generated from indentation Crack 13 Glass without ion implantation layer 15 Center position of ion implantation layer 16 Substrate surface

Claims (4)

  1. In a glass plate formed by implanting ions on the surface, the ions are nitrogen ions or silicon ions, the ion implantation depth is in the range of 10 nm to 10 μm from the surface, and the ion implantation amount is 1 × 10 12 ions. A glass plate having high fracture toughness characterized by being / cm 2 to 1 × 10 18 ions / cm 2 .
  2. The glass substrate having high fracture toughness according to any one of claims 1 to 5, wherein two or more ion implantation layers are formed.
  3. In ion implantation, injection current of the glass plate having high fracture toughness according to any one of claims 1 to 2, characterized in that implanting ions in the range of 0.05μA / cm 2 ~50μA / cm 2 It is a manufacturing method.
  4.   4. The method for producing a glass substrate having high fracture toughness according to claim 3, wherein the acceleration voltage at the time of ion implantation is continuously changed to change the thickness of the ion implantation layer.
JP2006063693A 2006-03-09 2006-03-09 Glass plate having high fracture toughness and method of manufacturing the same Pending JP2007238378A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104445998A (en) * 2014-11-25 2015-03-25 大连理工大学 Method for adjusting and controlling brittle-ductile transition thickness of brittle material in real time
JPWO2013051514A1 (en) * 2011-10-04 2015-03-30 旭硝子株式会社 cover glass
CN104556735A (en) * 2015-01-07 2015-04-29 大连理工大学 Atmospheric surface discharge plasma device for modifying surfaces of glass and polymer material
WO2017102345A1 (en) * 2015-12-18 2017-06-22 Agc Glass Europe Glass substrate for chemical strengthening and method for chemically strengthening with controlled curvature
WO2018005327A1 (en) * 2016-06-28 2018-01-04 Corning Incorporated Thin glass based article with high resistance to contact damage
EP3613711A1 (en) * 2018-08-21 2020-02-26 Schott AG Hollow body having a wall of glass with a surface region having contents of si and n
US10731403B2 (en) 2017-10-06 2020-08-04 Vkr Holding A/S Vacuum insulated glazing unit

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0323238A (en) * 1989-06-19 1991-01-31 Nippon Sheet Glass Co Ltd Surface modifying method for glass base material
JPH0585777A (en) * 1991-09-25 1993-04-06 Nippon Sheet Glass Co Ltd Glass substrate and production thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0323238A (en) * 1989-06-19 1991-01-31 Nippon Sheet Glass Co Ltd Surface modifying method for glass base material
JPH0585777A (en) * 1991-09-25 1993-04-06 Nippon Sheet Glass Co Ltd Glass substrate and production thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2013051514A1 (en) * 2011-10-04 2015-03-30 旭硝子株式会社 cover glass
CN104445998A (en) * 2014-11-25 2015-03-25 大连理工大学 Method for adjusting and controlling brittle-ductile transition thickness of brittle material in real time
CN104445998B (en) * 2014-11-25 2017-01-04 大连理工大学 A kind of real-time monitoring fragile material is crisp moulds the method changing thickness
CN104556735A (en) * 2015-01-07 2015-04-29 大连理工大学 Atmospheric surface discharge plasma device for modifying surfaces of glass and polymer material
WO2017102345A1 (en) * 2015-12-18 2017-06-22 Agc Glass Europe Glass substrate for chemical strengthening and method for chemically strengthening with controlled curvature
WO2018005327A1 (en) * 2016-06-28 2018-01-04 Corning Incorporated Thin glass based article with high resistance to contact damage
US10612129B2 (en) 2016-06-28 2020-04-07 Corning Incorporated Thin glass based article with high resistance to contact damage
US10731403B2 (en) 2017-10-06 2020-08-04 Vkr Holding A/S Vacuum insulated glazing unit
EP3613711A1 (en) * 2018-08-21 2020-02-26 Schott AG Hollow body having a wall of glass with a surface region having contents of si and n

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