WO2009067164A1 - Laser scoring of glass sheets at high speeds and with low residual stress - Google Patents
Laser scoring of glass sheets at high speeds and with low residual stress Download PDFInfo
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- WO2009067164A1 WO2009067164A1 PCT/US2008/012770 US2008012770W WO2009067164A1 WO 2009067164 A1 WO2009067164 A1 WO 2009067164A1 US 2008012770 W US2008012770 W US 2008012770W WO 2009067164 A1 WO2009067164 A1 WO 2009067164A1
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- Prior art keywords
- glass
- scoring
- laser beam
- glass sheet
- laser
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B33/00—Severing cooled glass
- C03B33/09—Severing cooled glass by thermal shock
- C03B33/091—Severing cooled glass by thermal shock using at least one focussed radiation beam, e.g. laser beam
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Definitions
- This invention relates to the laser scoring of glass sheets, such as the sheets used as substrates in the production of display devices, e.g., thin film transistor liquid crystal displays (TFT-LCDs).
- TFT-LCDs thin film transistor liquid crystal displays
- a median crack 115 also known as a partial vent or, simply, a vent
- a small initial flaw 111 is formed on the glass surface near one of its edges, which is then transformed into the vent by propagating laser light 121 formed into a beam 113 across the surface of the glass followed by a cooling area produced by a cooling nozzle 119. Heating of the glass with a laser beam and quenching it immediately thereafter with a coolant creates a thermal gradient and a corresponding stress field, which is responsible for the propagation of the vent.
- the scoring beam described in the '284 patent had a short elliptical shape with the longest axis of the beam being less than 10 times the material thickness.
- the length of the beam's long axis should not exceed 7mm.
- the scoring beam had an elongated elliptical shape with the longest axis preferably greater than 40mm.
- the beam was truncated from one or both ends, and as a result, the total length of the beam was reduced by 20-40%.
- a U-shape beam created by a scanning technique was used for scoring.
- Residual stress is a particularly significant problem in the case of glass sheets that are to be used as substrates in display devices.
- Many display devices such as TFT- LCD panels and organic light-emitting diode (OLED) panels, are made directly on glass substrates.
- OLED organic light-emitting diode
- a typical panel manufacturing process simultaneously produces multiple panels on a single substrate or a sub-piece of a substrate.
- the substrate is mechanically divided into parts along cut lines.
- Such mechanical cutting changes the stress distribution within the glass, specifically, the in-plane stress distribution seen when the glass is vacuumed flat. Even more particularly, the cutting relieves residual stresses in the sheet at the cut line since the cut edge is rendered traction free.
- Such stress relief in general results in changes in the vacuumed-flat shape of the glass sub-pieces, a phenomenon referred to by display manufacturers as "distortion.”
- the distortion problem is of substantial concern to display manufacturers and specifications regarding allowable distortion can be as low as 2 microns or less.
- the amount of distortion produced when such mechanical cutting is performed depends on the residual stress in the sheet, with lower levels of residual stress producing smaller distortions.
- the prior art relating to laser scoring is silent with regard to residual stress introduced into glass sheets during the scoring process.
- the prior art is also silent with regard to the distortion resulting from such residual stress when the glass sheets are subsequently mechanically cut during panel manufacturing processes.
- residual stress is also important in terms of the quality of the edges produced when a laser scored sheet of glass is divided into two sub-pieces.
- high levels of residual stress have been associated with edges having relatively low strength and poor quality, e.g., splinters and micro cracks.
- a third problem with the prior art techniques for performing laser scoring relates to the CTE of the glass being scored.
- Prior art laser scoring techniques have used glasses with relatively high CTE's, e.g., Corning Incorporated's Code 1737 LCD glass which has a CTE (0-300 0 C) above 37 x 10 '7 /°C. More recent glasses, e.g., Corning's EAGLE 2000® and EAGLE XGTM glasses, have lower CTE's. Higher CTE's, such as that of Code 1737 glass, translate into higher tensile stresses during heating which, all other things being equal, means that it easier to laser score such glasses at higher speeds.
- the lower CTE's of the more modern glass substrates used by the LCD industry result in much lower scoring speeds when conventional laser scoring technology is used.
- the invention provides a method of scoring a glass sheet (112) comprising: (a) translating (see arrow 17 in Fig. 1C) an elongated laser beam having a peak intensity Ipea k over a surface (114) of the glass sheet (1 12) at a speed S, said beam being characterized by an untruncated length Lo, where Lo equals the maximum distance along the length of the beam between locations at which the beam intensity at the surface (114) of the glass sheet (112), in the absence of any truncation, has fallen to 1/e 2 of Ipeak; and
- Ipea k and Lo are selected such that the translation of the laser beam over the surface (114) of the glass sheet (1 12) at the speed S produces a maximum temperature at the surface (114) of the glass sheet (112) that is less than or equal to the glass' strain point, the lowest possible temperature being preferred.
- a portion (23) of the beam proximal to the coolant area (15) is truncated (e.g., up to 20% of Lo is truncated).
- the coolant area (15) is preferably located within the portion of the beam that would have contacted the surface (114) of the glass sheet (112) if the beam had not been truncated.
- the invention provides a method of operating a laser scoring system in which a vent (115) is produced in a glass sheet (112) by translating a truncated laser beam (13) over a surface (114) of the sheet in tandem with a coolant area (15) which has a center point, said method comprising selecting the amount of truncation of the laser beam ( ⁇ ), or the distance (D) between the center point of the coolant area (15) and the nearest end of the laser beam prior to truncation, or both the amount of truncation ( ⁇ ) and the distance (D) between the center point of the coolant area and the nearest end of the laser beam prior to truncation to control at least one of (i) the depth of the vent (115) and (ii) the residual stress in sub-pieces produced from the sheet (112).
- the invention provides a method of operating a laser scoring system in which a vent (115) is produced in a glass sheet (112) by translating a truncated laser beam (13) over a surface (114) of the sheet in tandem with a coolant area (15) which has an outer edge, said truncation of the laser beam producing a truncated edge proximal to the coolant area (15), said method comprising:
- Figs. IA and IB are schematic diagrams of prior art scoring systems.
- Fig. 1C is a schematic diagram of an embodiment of the present invention.
- the reference number 17 in these figures represents the direction of scoring.
- Fig. 2 is a graph of calculated thermal histories of each point on a glass surface along a score line for different combinations of laser power and scoring speed for the case of a laser operating in dual mode.
- the laser beam had a length of 230 mm.
- Table 1 sets forth the laser powers and speeds for the various curves shown in this figure.
- the vertical axis in this figure shows temperature in C C and the horizontal axis shows time in seconds.
- the reference number 50 shows a maximum temperature limit and the reference number 60 shows a quenching area.
- Fig. 3 is a graph of calculated transient thermal stress versus the parameters ⁇ and D of Fig. 1C.
- Fig. 4 is a graph of vent depth versus the parameter ⁇ .
- the vertical axis shows vent depth in microns and the horizontal axis shows the degree of beam blockage ( ⁇ ) in millimeters.
- the triangular data points are measured values and the curve is a fit to those values.
- Fig. 5 is a graph of calculated exposure time (without quenching) versus scoring speed for a 60mm beam (curve 20), as well as for beams in accordance with the invention which have a length greater than 200mm, specifically, 250mm (curve 22) and
- 300mm (curve 24) in this figure.
- the vertical axis shows exposure time in seconds and the horizontal axis shows scoring speed in millimeters/second.
- the gap in the 60mm curve (its dashed portion) indicates the location of the maximum achievable scoring speed with a 60 mm beam, shown by the reference number 26 in this figure.
- Fig. 6 is a graph of measured peak glass surface temperatures produced by a representative beam of the invention (square data points) and a reference (comparative) beam (circular data points). The vertical axis shows peak glass surface temperature in
- Fig. 7 is a graph of measured peak residual stress generated during laser scoring by a representative beam of the invention (square data points) and a reference (comparative) beam (circular data points).
- the vertical axis shows peak residual stress in psi and the horizontal axis shows laser power in %. In this graph, higher laser powers correspond to higher scoring speeds.
- Fig. 8 is a graph of scoring speed versus laser power achieved without generating excessive residual stress for Coming's EAGLE 2000® (diamond-shaped data points) and EAGLE XGTM (square data points) LCD glasses.
- the vertical axis shows scoring speed in millimeters per second and the horizontal axis shows laser power in %.
- Fig. 9 is a schematic diagram of a prior art scoring system.
- Laser scoring is typically performed using a carbon dioxide laser operating at a wavelength of 10.6 ⁇ m. At this wavelength the absorption of oxide glasses can exceed 10 5 -10 6 l/m, which makes the effective penetration depth OfCO 2 radiation less than l-10 ⁇ m.
- the typical vent depth required for successful scoring has to be in the range of
- an Elongated Beam In accordance with the present invention, the above challenges are addressed and solved using a simpler solution which surprisingly has been found to effectively score glass sheets at high speeds with low levels of residual stress, including glass sheets composed of glasses having low coefficients of thermal expansion. That solution involves the use of a single elongated beam with an untruncated length Lo (see below) which is greater than or equal to 200 millimeters. Because of its long length, the beams used in the practice of the invention generally have large ratios of their major to minor axes, e.g., ratios greater than 130, preferably greater than 200, and most preferably greater than 300.
- a beam of this type results in a prolonged residence time on the surface of the glass during scoring which enables the creation of a deep vent even at scoring speeds exceeding 1000mm/s.
- the beam configuration and power distribution of the laser mode can be chosen to keep power density at a relatively low level enabling a consistent scoring process without overheating of the glass surface above the strain point of the glass being scored. This represents a clear advantage of the method since it means that high scoring speeds can be used without the generation of high levels of residual stress.
- the tensile stress generated during the scoring can be maximized by adjusting the relative position of the cooling zone and the trailing edge of the beam. This allows the temperature differential along the surface of the glass to be increased while holding the maximum temperature at the surface of the glass below the glass' strain point.
- laser scoring is performed using a non-symmetrical laser beam, e.g., a beam which has been truncated on just one end.
- the beam has a size (length) and power density which can be varied so as to accommodate different glass types and/or processing conditions (e.g., scoring speeds), although beams having a fixed size and power density can be used in the practice of the invention if desired, e.g., in connection with a dedicated scoring station used for a single type and thickness of glass.
- each point on the glass surface should experience the same thermal history determined by the following parameters: laser power and distribution of the power density within the laser beam; heating speed; maximum glass surface temperature achieved during heating; and quenching efficiency and location of the quenching zone.
- the scoring methods of the invention balance the system's process parameters such that a variation of one parameter is compensated by a variation of one or more other parameters so as to maintain essentially the same desirable thermal history for each point on the glass surface along the score line.
- the invention achieves high speed scoring with low residual stress by meeting the following conditions:
- the exposure of each point on the glass surface along the score line to laser radiation is sufficient to create a relatively deep vent, but, on the other hand, the duration of the exposure and the power density of the laser beam are selected so as not to cause overheating of the glass surface thus allowing the process to be run without inducing substantial amounts of residual stress; and (3) the location of the quenching zone within the trailing edge of the beam is chosen to maximize the thermal stress gradient for a given maximum glass surface temperature.
- FIG. 1 schematically illustrates the process of the '284 patent in Fig. IA, the process of the '220 patent in Fig. IB, and an embodiment of the present invention in Fig. 1C.
- the laser scoring processes described in the '284 and '220 patents include heating of the glass surface with a laser beam 113 of a limited size followed by a quenching zone or cooling area 15.
- a median crack or a partial vent
- a small initial flaw is first formed on the glass surface, which is then transformed into the vent and propagated by the laser beam and the quenching zone.
- the cooling area is positioned at some distance outside the beam boundaries (see Figs. IA and IB).
- IA and IB can achieve scoring, they are limited to speeds of 20mm/s-500mm/s depending on glass type. Any attempt to increase the scoring speed using the same configurations entails overheating of the glass which, in accordance with the invention, has been found to produce high residual stress levels as a result of the higher applied power densities. Moreover, the residual stress effect becomes more pronounced at higher scoring speeds, especially in the case of a low thermal expansion glass.
- Fig. 1C overcomes these problems by employing a significantly longer laser beam and, in accordance with the most preferred embodiments of the invention, by truncating one end of the beam to produce an asymmetrical beam footprint on the surface of the glass sheet.
- the scoring process can be described in terms of the tensile stress ⁇ produced in the glass during the scoring process.
- This tensile stress is proportional to ⁇ *E* ⁇ T, where ⁇ is the glass' linear thermal expansion coefficient (CTE), E is the glass' modulus of elasticity, and ⁇ T is a measure of the temperature difference on the glass' surface between the portion of the surface located under the laser beam and the portion located under the cooling nozzle.
- CTE glass' linear thermal expansion coefficient
- ⁇ T is a measure of the temperature difference on the glass' surface between the portion of the surface located under the laser beam and the portion located under the cooling nozzle.
- tensile stress ⁇ can be increased by heating the glass to a higher temperature.
- overheating of the glass close to or above its strain point causes glass ablation and entails the formation of irreversible high residual stress in the glass, which deteriorates the quality of the glass' edge, reduces its strength and makes for inconsistent operation of the scoring process.
- Fig. 2 shows the thermal history calculated for different combinations of laser power and speed using a beam length of 230mm. Table 1 lists the power levels and speeds for each of the curves shown in these figures.
- the glass properties used in the calculations of Fig. 2 correspond to those of Corning Incorporated's EAGLE 2000® glass. The figure also shows the areas where the cooling process takes place (quenching areas).
- the horizontal dotted line in this figure indicates the strain point of the glass used in performing these calculations, i.e., 666°C.
- this temperature represents an upper limit which should not be exceeded during scoring in order to avoid generation of excessive residual stress in the glass.
- lower maximum glass temperatures are preferred to higher maximum temperatures, assuming that heating of the glass surface and its subsequent quenching generate enough tensile stress to propagate the vent. In this way, the residual stress in the finished edge and sheet can be minimized.
- the calculated results of Fig. 2 show combinations of scoring parameters that can be successfully used without producing excessive residual stress as well as combinations (see reference numbers 100 and 110) that entail overheating of the glass (e.g., heating the glass so that T>666°C).
- the calculated results also show combinations of laser power and exposure time that can be used to run the process at reduced glass surface temperatures while still achieving a transient tensile stress level sufficient to create a vent (see reference numbers 70, 80, and 90). As shown below, these calculated results were confirmed experimentally.
- Fig. 3 The results of these calculations are shown in Fig. 3. As can be seen in this figure, for each distance D (i.e., the distance from the center of the coolant spot to the edge of the unblocked beam; see Fig. 1C), there is a range of ⁇ values (i.e., the length of the beam blockage; see Fig. 1C) over which the transient thermal stress has its highest values. These calculated results are qualitatively consistent with what was observed experimentally. Adjustment of ⁇ (and D) thus provides an effective approach for achieving sufficient tensile stress to produce a vent while not creating excessive levels of residual stress. Moreover, ⁇ also affects vent depth, with the depth being smaller for larger truncations (larger ⁇ values).
- vent depth has been found to be a non-linear function of ⁇ or, in other words, a non-linear function of the length b in Fig. 1C.
- This effect is shown in Fig. 4, where the upper part of this graph represents a suitable range of ⁇ values that have been found to work successfully in the scoring of 0.7 mm LCD glass.
- the non-linear behavior shown in Fig. 4 differs from that described in the '284, '220, and '875 patents, where a linear dependence of vent depth as a function of b (see Figs. IA and IB) was predicted.
- an elongated beam having an untruncated length Lo greater than or equal to 200 millimeters is used to perform the scoring.
- Lo b + ⁇ .
- Such a beam can provide an exposure time 3-5 times longer than that of a conventional laser scoring process at a scoring speed of 500mm/s. This enables heat transfer deep into the glass at a much higher scoring speed without overheating the glass surface. The vent depth created by such a beam can exceed 10% of the glass thickness even at a speed of
- L 0 will typically be about 300mm or less, although longer beams can be used if desired.
- the laser beam will typically be produced by a CO 2 laser, although other types of lasers can be used if desired.
- the beam will typically be passed through a beam expander and then elongated using cylindrical optics.
- the Lo value for an untruncated beam is determined using the 1/e 2 definition of beam length of the ISO 11146 standard. That is, the boundaries of the laser beam are defined as the locations at which beam intensity has fallen to 1/e 2 of its peak value Ip eak - According to this definition approximately 86% of the total beam energy is transmitted through the defined boundaries.
- the maximum temperature T max at the surface of the glass surface during scoring is kept below or at most equal to the glass' strain point T strain , i.e., the temperature at which the glass has a viscosity of 10 13 5 Pa*s (10 14 5 poise).
- T m a x ⁇ Tst r ai n - 60 and most preferably, T max ⁇ T strain - 100, where T max and T strain are in 0 C.
- the maximum glass temperature can be below (T str ai n - 150) or even (T stram - 200).
- the glass temperature can be measured in various ways, a preferred procedure being through the use of a thermal imaging (thermal vision) camera.
- the peak residual stress in sub-pieces produced from the glass sheet is less than or equal to 300 psi and most preferably, less than or equal to 100 psi.
- peak residual stresses above 300 psi can be tolerated, e.g., stresses ranging up to 500 psi.
- higher stress levels may be acceptable if the glass sheet is not likely to undergo significant additional edge stresses.
- distortion in the body of the sheet is likely to be small because of the sheet's large size even for a high peak value at an edge.
- the peak residual stress in a scored and separated sheet is preferably measured using a birefringence technique.
- the invention can be practiced using an untruncated beam but preferably employs a beam which has been truncated on one end, i.e., its trailing end closest to (proximal to) the coolant area.
- the truncation can be performed using a shield specifically constructed for this purpose.
- a portion of the nozzle assembly used to apply coolant to the sheet can be positioned to intercept and thus truncate the trailing part of the beam. This latter approach is illustrated in Fig. 1C where the untruncated beam 21 is intercepted by the housing of nozzle 19 and thus becomes truncated beam 13 at the surface of the glass.
- the degree of beam blockage in accordance with the present invention preferably does not exceed approximately 20% of the total beam length. Also, again unlike the '875 patent, the degree of beam blockage is preferably selected depending on the desired scoring speed.
- the experimental data was obtained using a circular polarized CO 2 laser beam which was passed through a variable beam expander and then was transformed into an elongated beam using cylindrical optics.
- the optical system allowed the length of the beam to be adjusted along the scoring direction to obtain untruncated lengths Lo equal to or greater than 200 mm.
- the coolant jet was positioned to contact the glass sheet inside the trailing edge of the untruncated beam. As shown in Fig. 1C, the beam was truncated using the body of the nozzle.
- Fig. 6 compares the peak surface temperature of the glass produced by a beam of the invention (square data points) with that produced by a reference beam (circular data points).
- the beam of the invention had an untruncated length of 200 mm and was truncated by 10-15 mm while the reference beam had an untruncated length of 100 mm and was used without truncation.
- the distance L (see Fig. 1) was in each case equal to 3-6 mm.
- the glass used in these experiments was Coming's EAGLE 2000® glass. The surface temperatures of the glass were measured using a thermal-vision camera. In this figure, higher laser powers correspond to higher scoring speeds.
- the surface temperature rapidly climbs above 700 0 C at relative laser power levels exceeding 30%.
- the surface temperature stays below the glass strain point, even when the relative laser power exceeds 60%. From the point of view of scoring speed, this and related experiments demonstrated that use of the reference beam can easily cause an overheating of the glass surface with glass temperature raising well above 600 0 C when the scoring speed just exceeds 450- 500mm/sec, whereas when the beam of the invention is used, the maximum glass temperature remains below 600 0 C even when the scoring speed approaches lOOOmm/sec. The invention thus permits laser scoring to be performed at higher speeds without overheating of the glass.
- Fig. 7 sets forth measured peak residual stress in the separated sub-pieces resulting from scoring with the reference (circular data points) and inventive (square data points) beams described above.
- the scoring speeds are also shown in this figure.
- the reference beam results in stress levels well above the 500 psi level once the scoring speed exceeds 500 mm/sec while the beam of the invention remains well below this level even at speeds of 1000 mm/sec.
- Fig. 8 illustrates the ability of the laser beam of the invention to score glass substrates having low CTE's.
- the same laser beam was used as in generating the square data points of Figs. 6 and 7.
- the diamond-shaped data points in Fig. 8 are for Coming's EAGLE 2000® glass while the square data points are for Coming's EAGLE XQ TM gi ass .
- the laser beam of the invention successfully scored substrates composed of these low CTE glasses at laser power levels corresponding to speeds well-above 500 mm/sec, e.g., 750-1000mm/s.
- the resulting sub-pieces had low levels of residual stress, i.e., levels typically less than or equal to 100 psi. Breaking of the glass sheets scored in this manner was completed by glass bending or by using a no-bend, ultrasonic separation method.
- the use of an elongated laser beam in combination with partial blockage of the beam's trailing edge allows for effective scoring of glass sheets.
- the combination allows the quenching location to be selected so as to maximize the vent depth and also to maximize the thermal stress gradient generated during the scoring without increasing the maximum glass surface temperature.
- the technique allows high scoring speeds, e.g., speeds equal to or above 750-1000mm/s, to be achieved without adding residual stress even for glass substrates having low CTEs.
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Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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CN2008801253132A CN101910077B (en) | 2007-11-20 | 2008-11-14 | Laser scoring of glass sheets at high speeds and with low residual stress |
JP2010534946A JP5416127B2 (en) | 2007-11-20 | 2008-11-14 | High speed / low residual stress laser scoring of glass sheets |
Applications Claiming Priority (2)
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US373807P | 2007-11-20 | 2007-11-20 | |
US61/003,738 | 2007-11-20 |
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WO2009067164A1 true WO2009067164A1 (en) | 2009-05-28 |
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US (1) | US8011207B2 (en) |
JP (1) | JP5416127B2 (en) |
KR (1) | KR101469304B1 (en) |
CN (1) | CN101910077B (en) |
TW (1) | TWI388523B (en) |
WO (1) | WO2009067164A1 (en) |
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- 2008-01-15 US US12/008,949 patent/US8011207B2/en not_active Expired - Fee Related
- 2008-11-14 WO PCT/US2008/012770 patent/WO2009067164A1/en active Application Filing
- 2008-11-14 JP JP2010534946A patent/JP5416127B2/en not_active Expired - Fee Related
- 2008-11-14 CN CN2008801253132A patent/CN101910077B/en not_active Expired - Fee Related
- 2008-11-14 KR KR1020107013555A patent/KR101469304B1/en active IP Right Grant
- 2008-11-18 TW TW097144611A patent/TWI388523B/en not_active IP Right Cessation
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US6237875B1 (en) * | 1998-08-18 | 2001-05-29 | Daimlerchrysler Ag | Airbag payload landing system for damping landing impact forces on a flying payload |
US6489588B1 (en) * | 1999-11-24 | 2002-12-03 | Applied Photonics, Inc. | Method and apparatus for separating non-metallic materials |
US6829910B1 (en) * | 2000-04-25 | 2004-12-14 | Asahi Glass Company, Ltd. | Removal of enclosed glass parts after cutting using heating and cooling techniques |
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JP2010111568A (en) * | 2008-09-29 | 2010-05-20 | Corning Inc | Laser separation method of glass sheet |
US8171753B2 (en) | 2009-11-18 | 2012-05-08 | Corning Incorporated | Method for cutting a brittle material |
US9027815B2 (en) | 2010-08-31 | 2015-05-12 | Corning Incorporated | Apparatus and method for making glass sheet with improved sheet stability |
US8887529B2 (en) | 2010-10-29 | 2014-11-18 | Corning Incorporated | Method and apparatus for cutting glass ribbon |
Also Published As
Publication number | Publication date |
---|---|
US8011207B2 (en) | 2011-09-06 |
KR20100101605A (en) | 2010-09-17 |
JP2011502948A (en) | 2011-01-27 |
CN101910077B (en) | 2013-08-07 |
US20090126403A1 (en) | 2009-05-21 |
KR101469304B1 (en) | 2014-12-05 |
TW200940464A (en) | 2009-10-01 |
TWI388523B (en) | 2013-03-11 |
CN101910077A (en) | 2010-12-08 |
JP5416127B2 (en) | 2014-02-12 |
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