WO2010059907A1 - Laser assisted frit sealing of high cte glasses and the resulting sealed glass package - Google Patents

Laser assisted frit sealing of high cte glasses and the resulting sealed glass package Download PDF

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Publication number
WO2010059907A1
WO2010059907A1 PCT/US2009/065271 US2009065271W WO2010059907A1 WO 2010059907 A1 WO2010059907 A1 WO 2010059907A1 US 2009065271 W US2009065271 W US 2009065271W WO 2010059907 A1 WO2010059907 A1 WO 2010059907A1
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WO
WIPO (PCT)
Prior art keywords
glass plate
frit
glass
sealing
cte
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PCT/US2009/065271
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English (en)
French (fr)
Inventor
Stephan L Logunov
Sasha Marjanovic
Original Assignee
Corning Incorporated
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Filing date
Publication date
Application filed by Corning Incorporated filed Critical Corning Incorporated
Priority to CN200980153150.3A priority Critical patent/CN102264662B/zh
Priority to KR1020117014717A priority patent/KR101530753B1/ko
Priority to EP09761112A priority patent/EP2370372A1/en
Priority to JP2011537643A priority patent/JP2012509830A/ja
Publication of WO2010059907A1 publication Critical patent/WO2010059907A1/en

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Classifications

    • 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
    • C03C27/00Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06Joining glass to glass by processes other than fusing
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/06Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving heating of the applied adhesive
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00Organic light-emitting devices
    • H10K50/80Constructional details
    • H10K50/84Passivation; Containers; Encapsulations
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00Organic light-emitting devices
    • H10K50/80Constructional details
    • H10K50/85Arrangements for extracting light from the devices
    • H10K50/858Arrangements for extracting light from the devices comprising refractive means, e.g. lenses
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2101/00Properties of the organic materials covered by group H10K85/00
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00Organic light-emitting devices
    • H10K50/80Constructional details
    • H10K50/84Passivation; Containers; Encapsulations
    • H10K50/841Self-supporting sealing arrangements
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00Organic light-emitting devices
    • H10K50/80Constructional details
    • H10K50/84Passivation; Containers; Encapsulations
    • H10K50/842Containers
    • H10K50/8426Peripheral sealing arrangements, e.g. adhesives, sealants

Definitions

  • the present invention relates to a laser assisted frit sealing method used to manufacture a glass package having a first glass plate (with a relatively high CTE of about 80-9OxIO "7 0 C "1 ), a second glass plate, and a frit (with a CTE that is at least about 35XlO -7 0 C "1 ), where the frit forms a seal (e.g., hermetic seal) which connects the first glass plate to the second glass plate.
  • a seal e.g., hermetic seal
  • Encapsulation of moisture and oxygen sensitive devices is an important part of manufacturing Organic Light Emitting Diode (OLED) displays. It has been shown that laser assisted frit sealing of OLEDs between two display glass plates, which have a moderate coefficient of thermal expansion (CTE) of about 30-4OxIO "7 0 C "1 that are separated by a frit, is feasible at a high speed up to 20-50 mrn/s. The relatively high sealing speed up to 20-50 mm/s is an important requirement for enabling a cost efficient manufacturing process.
  • This laser assisted frit sealing process has been described in co-assigned U.S. Patent Application Publication No. 2007/0128966 entitled “Method of Encapsulating a Display Element” and co- assigned U.S. Patent Application Publication No. 2007/0128967 entitled “Method of Making a Glass Envelope”. The contents of these two documents are hereby incorporated by reference herein.
  • inventions of the present invention are directed to a glass package and methods of making the glass package.
  • the glass package may be, for example, a glass package containing an electronic component such as an electro-optic component.
  • the glass package may include one or more layers of an organic material such as an organic electro-luminescent material.
  • the glass package may comprise a display device, such as an organic light emitting diode (OLED) display, or the glass package may comprise a photovoltaic device (e.g. solar cell).
  • OLED organic light emitting diode
  • embodiments of the present invention include a glass package including: (a) a first glass plate which has a CTE in a range of about 80-9OxIO "7 0 C "1 ; (b) a second glass plate; and (c) a frit which has a CTE which is at least about 35xlO "7 0 C "1 , where the frit forms a seal which connects the first glass plate to the second glass plate.
  • embodiments of the present invention include a method for manufacturing a glass package including the steps of: (a) providing a first glass plate, where the first glass plate has a CTE in a range of about 80-9OxIO "7 0 C "1 ; (b) providing a second glass plate; (c) providing a frit, where the frit has a CTE that is at least about 35xlO "7 0 C "1 ; (d) depositing the frit onto the first glass plate or the second glass plate; (e) placing the first glass plate on the second glass plate where the frit is located between the first glass plate and the second glass plate; and (f) using a laser to direct a laser beam through the first glass plate or the second glass plate towards the frit and then moving the laser beam at a predetermined sealing speed along the frit to heat the frit such that the frit melts and forms a seal which connects the first glass plate to the second glass plate, where the laser beam forms a footprint on the frit and has a
  • FIGURES IA and IB respectively show a cross-sectional side view and a top view that illustrate the basic components of a sealing device and a sealed glass package in accordance with an embodiment of the present invention
  • FIGURE 2 is a flowchart illustrating the steps of an exemplary sealing method for manufacturing the glass package shown in FIGURES IA and IB in accordance with an embodiment of the present invention.
  • FIGURES 3-9 are diagrams and plots which are used to illustrate the results of various experiments that where conducted to test the sealing method and glass package in accordance with an embodiment of the present invention. DETAILED DESCRIPTION
  • the laser assisted frit sealing techniques of the present invention are described below with respect to manufacturing a basic glass package, it should be understood that the same or similar laser assisted frit sealing techniques can be used to seal two glass plates (at least one of which has a relatively high CTE of about 80-9OxIO "7 0 C "1 ) to one another, which can be used in a wide variety of applications and devices such as solid state lighting, solar cells and even hermetically sealed OLED displays, for example. Accordingly, the glass package and laser assisted frit sealing technique of the present invention should not be construed in a limited manner.
  • the sealed glass package 100 includes a first glass plate 102 (which has a CTE in a range of about 80-9OxIO "7 0 C "1 ), one or more components 104, electrodes 106 (optional), a frit 108 (which has a CTE that is at least about 35xlO "7 0 C "1 ), and a second glass plate 110.
  • the sealed glass package 100 has a seal 112 (e.g., hermetic seal 112) formed from the frit 108 which protects the one or more components 104 (if present) located between the first glass plate 102 and the second glass plate 110.
  • the electrode(s) 106 (if present) are connected to the component(s) 104 and also pass through the seal 112 so they can be connected to an external device (not shown).
  • the seal 112 is typically located around the perimeter of the glass package 100 such that the component(s) 104 (if present) and at least a part of the electrode(s) 106 (if present) are located within the perimeter of the seal 112.
  • seal 112 is formed by melting the frit 108 and the ancillary components such as a sealing device 114 (e.g., laser 114) which are used to heat and melt the frit 108 to form the seal 112 (e.g., hermetic seal 112) are described in greater detail below with respect to FIGURE 2 and the experimental results section.
  • a sealing device 114 e.g., laser 114
  • hermetic seal 112 e.g., hermetic seal 112
  • FIGURE 2 there is a flowchart illustrating the steps of an exemplary sealing method 200 for manufacturing the sealed glass package 100 in accordance with the present invention.
  • the first glass plate 102 and the second glass plate 110 are provided so that one can make the sealed glass package 100.
  • the first and second glass plates 102 and 110 are glass plates such as soda lime glass plates and both have CTEs in a range of about 80-9OxIO "7 0 C "1 .
  • the first glass plate 102 (or second glass plate 110) is a glass plate such as a soda lime glass plate and has a CTE in a range of about 80-9OxIO "7 0 C "1 while the second glass plate 110 (or the first glass plate 102) is a glass plate which has a CTE that is about 30xl0 "7 0 C "1 or less than the CTE of the first glass plate 102 (or second glass plate 110).
  • the second glass plate 110 which has the CTE that is about 30xl0 "7 0 C "1 or less than the CTE of the first glass plate 102 (or second glass plate 110) can include alkaline- earth aluminoborosilicate glass plates like the ones manufactured and sold by Corning Incorporated under the brand names of Code 1737 glass or Eagle2000TM glass or it can be like the glass plates manufactured and sold by companies like Asahi Glass Co. (e.g., OAlO glass and OA21 glass), Nippon Electric Glass Co., NHTechno and Samsung Corning Precision Glass Co. (for example).
  • Asahi Glass Co. e.g., OAlO glass and OA21 glass
  • Nippon Electric Glass Co. NHTechno and Samsung Corning Precision Glass Co. (for example).
  • the frit 108 (e.g., frit paste 108) which has a CTE that is at least about 35xlO "7 0 C "1 is provided and deposited along the edges of the first glass plate 102 (or the second glass plate 110) in a manner that the frit 108 forms a closed-loop on a surface of the first glass plate 102 (or the second glass plate 110).
  • the frit 108 can be placed approximately 1 mm away from the free edges of the first glass plate 102 (or the second glass plate 110).
  • the frit 108 has a CTE that does not match the CTE(s) of at least one of the glass plates 102 and 110.
  • the frit 108 is a low temperature glass frit that contains one or more absorbing ions (e.g., transition metals) chosen from the group including iron, copper, vanadium, and neodymium (for example).
  • the frit 108 may also be doped with a filler (e.g., inversion filler, additive filler) to lower the CTE to at least about 35xlO "7 0 C "1 .
  • the frit 108 could have a composition of Sb 2 O 3 (23.5 mole %), V 2 O 5 (47.5 mole %), P 2 O 5 (27 mole %), TiO 2 (1.0 mole %), Al 2 O 3 (1.0 mole %), Fe 2 O 3 (2.5 mole %), and at least 10% of a ⁇ -eucryptite glass-ceramic CTE lowering filler (LiAlSiO 4 ).
  • the compositions of these frits 108 and several different exemplary frits 108 which could be used in the present invention are discussed in detail in co-assigned U.S. Provisional Patent Application Serial No.61/084,007, filed July 28, 2008, and co-assigned U.S. Patent No. 6,998,776 entitled "Glass Package that is Hermetically Sealed with a Frit and Method of Fabrication". The contents of these documents are hereby incorporated by reference herein.
  • the frit 108 could be pre-sintered to the first glass plate 102 (or second glass plate 110).
  • the frit 108 which was deposited onto the first glass plate 102 (or second glass plate 110) would be heated so that it becomes attached to the first glass plate 102 (or second glass plate 110).
  • the pre-sintering step 208 can be performed by placing the first glass plate 102 and the deposited frit 108 into a furnace where they are heated at 400 0 C for 1 hour and then cooled at a controlled rate to prevent the cracldng of the frit 108 and the first glass plate 102.
  • the pre-sintered frit 108 can be ground to reduce its thickness variation to less than 5-10 ⁇ m (for example).
  • the components 104 and associated electrodes 106 are deposited onto the second glass plate 110 (or first glass plate 102).
  • the components 104 and associated electrodes 106 can be associated with OLEDs, solid state lighting, and solar cells.
  • the glass package 100 can contain a liquid (not shown) instead of or in addition to the components 104 and electrodes 106.
  • the first glass plate 102 is placed on the second glass plate 110 where the frit 108 is located between the first glass plate 102 and the second glass plate 110.
  • the second glass plate 110 can be placed on the first glass plate 102 where the frit 108 is located between the first glass plate 102 and the second glass plate 110.
  • the frit 108 is heated by using the sealing device 114 (e.g., laser 114) in a manner such that the frit 108 forms the seal 112 (e.g., hermetic seal 112) which bonds the first glass plate 102 to second glass plate 110 (see FIGURE IB).
  • the seal 112 would protect the component(s) 104 (if any) by preventing, for example, oxygen and moisture located within the ambient environment from entering into the sealed glass package 100.
  • the sealing device 114 (laser 114) directs a laser beam 115 through the first glass plate 102 or the second glass plate 110 (shown) towards the frit 108 and then moves the laser beam 115 at a predetermined sealing speed (e.g., 20-50 mm/s) along the frit 108 to heat the frit 108 such that the frit 108 melts and forms a seal 112 which connects the first glass plate 102 to the second glass plate 110.
  • the laser beam 115 would typically have a spot size that is greater than a width of the frit 108.
  • the width of the frit 108 may be at least 1 mm, hence suitable spot sizes for the laser beam can exceed 1 mm, such as, for example, a beam size of at least about 2 mm, at least about 3 mm or at least about 4 mm in diameter.
  • the laser beam 115 would form a footprint on the frit 108 and have a residence time on a given point of the frit 108 within the footprint which is equal to or greater than 100 msec, equal to or greater than 200 msec, or even equal to or greater than 400 msec (note: the spot size and footprint can be related to e.g. 1/e 2 , full width max (FWHM) etc.).
  • the > 100 msec residence time of the laser beam 115 on a given point of the frit 108 during the sealing process is desirable since this helps prevent cracking and delamination of the frit 108 from the first and second glass plates 102 and 110.
  • a detailed discussion about the sealing step 216 and the residence heating time (heating profile) is provided below in the experimental results section.
  • the sealing device 114 e.g., laser 114 can be used to emit a light 115 (e.g., laser beam 115) that heats the frit 108 in a manner where the temperature of the frit 108 is raised to a substantially constant temperature as the light 115 is moved along the frit 108 (e.g. along a sealing line 118) that has regions free of electrodes 106 and regions occupied by electrodes 106 (if used) while the frit 108 melts and forms the seal 112 which connects the first glass plate 102 to the second glass plate 110.
  • Examples of different sealing techniques and set-ups that can be used to enable a constant temperature sealing technique in the present invention have been described in detail in co-assigned U.S. Patent No. 7,371,143 entitled "Optimization of Parameters for Sealing Organic Emitting Light Diode (OLED) Displays". The contents of this document are hereby incorporated by reference herein.
  • the calcium patch 302 may be used, for example, to detect leakage of the package (non-hermeticity), and thus can serve as a surrogate for sensitive package contents.
  • the calcium patch 302 can represent the one or more organic layers of an OLED device, and the results of a calcium patch test can be used to determine the effects from a given seal on the OLED device. All or a portion of the calcium patch 302 turning to a "white flaky crust" after a predetermined length of time can be used to indicate the presence of oxygen in the package and potential leakage of the package.
  • the inventors experimented with different sealing conditions by varying the laser power, the sealing speed and the beam size.
  • the inventors experimented with different types of frits 108 including ones with the 30% ⁇ -eucryptite filler as well as frits 108 with different amounts of glass to ⁇ -eucryptite filler ratio, ranging from 70/30 to 90/10.
  • soda-lime glass plates 102 and 110 sealed well with a 1 mm wide frit 108 at a slow speed 2 mm/s with a laser power 33 watts and an expanded beam spot size 3.2 mm, while very high sealing yields could be obtained with Eagle2000® glass plates and 1 mm wide frits 108 using the same sealing conditions but with a sealing speed of 20 mm/s and beam spot size of 1.8 mm.
  • the sealing results with soda-lime glass plates 102 and 110 where very poor at sealing conditions of laser power 33 W 5 sealing speed 20 mm/s and beam spot size of 1.8 mm.
  • a problem that this present invention solves is that typical residence heating time for high CTE glasses, 80-9OxIO "7 0 C "1 should be at least an order of magnitude higher than in the case of display glasses to prevent cracking and delamination of the frit 108 from the first and second glass plates 102 and 110 (see discussion below).
  • Frit 108 Sb 2 O 3 (23.5 mole %), V 2 O 5 (47.5 mole %), P 2 O 5 (27 mole %), TiO 2 (1.0 mole %), Al 2 O 3 (1.0 mole %), Fe 2 O 3 (2.5 mole %), and at least 10% of a ⁇ -eucryptite glass-ceramic CTE lowering filler (LiAlSiO 4 ). » Other glasses from TABLE #1 are all Coming's commercially available glasses.
  • Eagle 2000TM glass is an alkaline earth boroaluminosilicate display glass with CTE of
  • Glasses A and B are lime aluminosilicate glasses, with CTEs of 5IxIO "7 0 C “1 and 59xlO "7 0 C “1 , respectively.
  • Glass C is an alkali-zinc borosilicate glass, commercially available as microscope cover glass with CTE of 74x10 " 0 C " .
  • FIGURE [[5]] 3 there is a plot illustrating the heating profiles of multiple high CTE glass packages 100 as a function of sealing speed or laser beam shape change in accordance with an embodiment of the present invention.
  • the x-axis is time (seconds)
  • the y-axis is frit temperature (°C)
  • the following numbering scheme is used to identify the various curves:
  • This solid line indicates the intrinsic rate of glass cooling. 2. This solid line indicates the heating profile when sealing at 2 mm/s with a spot size of 3.2 mm while being measured at the center of the 0.7 mm wide frit 108.
  • This dashed line indicates the heating profile when sealing at 2 mm/s with a spot size of 3.2 mm while being measured on an edge of the 0.7 mm wide frit 108.
  • This solid line indicates the heating profile when sealing at 2 mm/s with a spot size of 1.8 mm while being measured at the center of the 0.7 mm wide frit 108.
  • This dashed line indicates the heating profile when sealing at 2 mm/s with a spot size of 1.8 mm while being measured on an edge of the 0.7 mm wide frit 108.
  • This solid line indicates the heating profile when sealing at 20 mm/s with a spot size of 1.8 mm while being measured at the center of the 0.7 mm wide frit 108.
  • This dashed line indicates the heating profile when sealing at 20 mm/s with a spot size of 1.8 mm while being measured on an edge of the 0.7 mm wide frit 108.
  • TABLE #1 and FIGURE 3 indicate a wider laser beam 115 spot size provides more uniform heating profile, which is important for laser frit sealing of high CTE glass like soda-lime.
  • the inventors put together a setup which measures the in-situ birefringence in the sealed glass packages 100.
  • the setup is similar to the Tardy method that was described in an article by M.H.L. Tardy "An Experimental Method for Measuring the Birefringence in Optical Materials", Optics Review, vol. 8, pages 59-69, 1929 (the contents of which are incorporated by reference herein).
  • the inventors monitored the birefringence by using a setup with a fast video camera. This enabled the inventors to calculate the transient stress, and residual stress in the sealed glass packages 100.
  • a birefringence map was produced for two tested glass packages, each of which was made from 0.63 mm thick soda-lime glass plates 102 and 110 with a typical 1 mm wide frit 108 located there between, where the tested first glass package was sealed at 10 mm/s with a 1.8 mm spot laser beam 115 and laser power of 20 watts, and the tested second glass package 100b was sealed at 2 mm/s with a 1.8 mm spot laser beam 115 and laser power of 12 watts.
  • the level of stress in the 10 mm/s sealed first glass package was significantly higher than the stress in the 2 mm/s sealed second glass package (see FIGURE 6).
  • the inventors used the same sealed second glass package to compare the residual birefringence obtained from the setup 600 with the residual birefringence obtained from a standard calibrated polarimeter.
  • the birefringence was also measured perpendicular to typical frits 108 in several soda-lime glass packages 100 and the data that was collected on a Hinds polaroscope is shown in the plot of FIGURE [[7]] 4. In this plot, the x-axis is distance across the frit (mm), the y-axis is birefringence (nm/cm), and the following numbering scheme is used to identify the various curves:
  • This soda-lime glass package 100 was sealed using a mask at 20 mm/s with laser power 175 watt and laser beam spot size of 4.8 mm.
  • This soda-lime glass package 100 was sealed using a mask at 20 mm/s with laser power 370 watt and laser beam spot size of 6.4 mm.
  • This soda-lime glass package 100 was sealed using a mask at 20 mm/s with laser power 18 watt and laser beam spot size of 1.6 mm.
  • a traditional Eagle 2000TM glass package sealed with a laser power of 33 watts, laser beam spot size of 1.8 mm and sealing speed 20 mm/s produced stress that was comparable with the soda-lime glass package 100 which was sealed with laser power of 370 watts, laser beam spot size of 6.4 mm and sealing speed of 20 mm/s. It should be appreciated that the lower the stress then the better the mechanical performance and lifetime of the glass package 100.
  • Hinds polaroscope provides values of birefringence that give an idea about the peak value of stress in the frit 108, and the width of the stress relative to the width of the frit 108.
  • the resulting birefringence shown in the plot of FIGURE 4, could be converted to stress values with known stress-optical coefficients as shown in FIGURE 5 when certain assumptions are made about the stress localization along the optical path.
  • the x-axis is distance (mm)
  • the y-axis is stress (psi) in soda-lime glass packages 100
  • the following numbering scheme is used to identify curves associated with sealing conditions: (1) 2 mm/s sealing speed, laser power of 12 watts, laser beam spot size 1.8 mm; and (2) 10 mm/s sealing speed, laser power of 20 watts, laser beam spot size 1.8 mm. Since, it is possible to monitor stress during sealing at any given point of time, peak stress values could be obtained for both transient and residual stresses. This data is summarized in FIGURE 9.
  • FIGURE 6 there is a graph that summarizes peak stresses for different glasses packages and sealing conditions including both the transient stress (bottom diagonal hatching) and residual stresses (top diagonal hatching).
  • the x-axis indicates multiple sampled glass packages
  • the y-axis is maximum stress (psi)
  • the samples are identified as follows: (1) Eagle stands for Eagle 2000TM glass plates sealed with typical frit 108; (2) SLN stands for soda-lime glass plates 102 and 110 sealed with typical frit 108; and (3) SL90-10 refers to soda-lime glass plates 102 and 110 sealed with typical frit 108 which contains a 90/10 glass to CTE lowering filler ratio (note: the second number is related to laser sealing speed 2 mm/s or 10 mm/s).
  • the sealing conditions included laser power of 12 and 20 watts (for 2 and 10 mm/s, respectively), and laser beam spot size of 1.8 mm.
  • the value of transient stress was found to be higher for soda-lime glasses than for Eagle 2000TM glass, but the peak value of the stress did not significantly change with different sealing speeds.
  • the residual stress values dropped when the sealing was done at slower speed for soda-lime glass.
  • the difference between Eagle 2000TM glass and soda-lime glass sealing was most noticeable for residual stress values, as shown in FIGURES 4 and 6.
  • the amount of residual stress in the glass package 100 should not exceed typical stress values in the traditional glass package by 4-5 times.
  • the amount of maximum residual stress in the glass package 100 was found to be less than 1500 psi, therefore for the traditional glass package it should be less than 7000 psi.
  • the residual stress in the glass package 100 should not be more than about 1500 psi, and for the traditional glass package it should not to be more than 7000 psi.
  • the difference in stress from the backplane glass and cover glass should be less than 20-30%. Effects of the laser beam spot size
  • the residence heating time the time needed for frit to heat up, seal and cool down (see also step 216 in FIGURE 2) and the uniformity of the heating for the center and edge of the frit 108.
  • Uniform heating of the frit 108 ensures that the center and edge of the frit 108 have similar residence heating time.
  • the difference in the residence heating time for the center of the lmm wide frit 108 for a 1.8 mm wide beam and 1 mm/s speed (12 W power) will be 1.8 sec, while for a 3.25 mm wide beam and 2 mm/s (30 W power) it is almost the same ( ⁇ 1.6 sec), but the sealing results for a 3.25 mm wide beam was much better.
  • the residence heating time for the edge of the frit 108 will be much shorter for a 1.8 mm beam (than for 3.25 mm beam).
  • the laser beam may have an intensity profile (distribution of intensity across the width of the beam) that is step-like, having a substantially uniform intensity across the width of the beam, or the beam may have a Gaussian intensity profile.
  • a substantially uniform intensity distribution suggests that some small variation in intensity across the width of the beam is possible. For example, in practice a true step function intensity distribution is very difficult to achieve, and some slope to the "sides" of the distribution, or other small variations in intensity may occur.
  • Typical seals 112 that protect Ca patches 302 (for hermeticity tests) in a glass package 100 made with a 2 mm/s sealing speed have been discussed above (made with two soda-lime glass plates 102 and 110 and a 1 mm wide frit 108 which sealed a Ca patch 302 using sealing conditions of laser power 33 W, sealing speed 2 mm/s, and an expanded beam spot size 3.2 mm).
  • the laser beam 115 spot size can be increased to maintain the same heating profile as for lower speeds. This was demonstrated with a 400 W laser power, sealing speed of 20 mm/s, and the laser beam spot size of 9 mm. Due to the limited number of these types of glass packages 100 prepared there is no statistical data, but at least two of these glass packages 100 successfully sealed a Ca patch 302 and survived at least 2000 hours in a lab environment. This suggests that sealing of high CTE glasses can be enabled by maintaining a wide heating profile. This approach allows an increase of the residence heating time across the width of the frit 108 while maintaining the relatively high sealing speed of 20 mm/s. Frit modifications
  • strain point is lower than the sealing temperature, then the stress would be lower for a lower strain point glass. This was the case for glasses A and B where glass A with a strain point of 472 0 C sealed well to Eagle 2000TM glass, while glass B which had a similar CTE but had a strain point above 800 0 C did not seal at all — instead, it delaminated.
  • the overall value of strain CTE* ⁇ T/ ⁇ t should be lower than a certain value.
  • a typical value for producing a good seal is —1500 ppm. However, this number can be exceeded if the glass is cooled slower than its intrinsic cooling rate.
  • a strain point of the glass plate 102 and 110 minus an equilibrated temperature of the glass plate 102 and/or 110 before the sealing process can be less than 500°C at a given residence heating time (e.g. >400 msec).
  • a residence heating time e.g. >400 msec
  • the ⁇ T between strain point and ambient temperature has to be decreased by raising the ambient temperature.
  • the ambient temperature may need to be increased at least by 200 °C or 100 0 C, respectively.
  • a strain point of the glass plate 102 and 110 minus an equilibrated temperature of the glass plate 102 and/or 110 before the sealing process can be less than about 400°C at a given residence heating time equal or greater than about 200 msec.
  • a strain point of the glass plate 102 and 110 minus an equilibrated temperature of the glass plate 102 and/or 110 before the sealing process can be less than about 300°C at a given residence heating time equal to or greater than about 100 msec.
  • the thickness of the glass plates 102 and 110 also plays an important role in glass sealing.
  • Glass C with a thickness of 150 ⁇ m, could be sealed to Eagle 2000TM glass, while the thicker glasses C 5 >400 ⁇ m, developed cracks and delamination at the sealing conditions described above with respect to TABLE #1.

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  • Materials Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Physics & Mathematics (AREA)
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  • Joining Of Glass To Other Materials (AREA)
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PCT/US2009/065271 2008-11-24 2009-11-20 Laser assisted frit sealing of high cte glasses and the resulting sealed glass package WO2010059907A1 (en)

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CN200980153150.3A CN102264662B (zh) 2008-11-24 2009-11-20 高cte玻璃的激光辅助的玻璃料密封以及制得的密封的玻璃封装
KR1020117014717A KR101530753B1 (ko) 2008-11-24 2009-11-20 높은 열팽창계수 글래스의 레이저 이용 프릿 밀봉 및 이에 따른 밀봉 글래스 패키지
EP09761112A EP2370372A1 (en) 2008-11-24 2009-11-20 Laser assisted frit sealing of high cte glasses and the resulting sealed glass package
JP2011537643A JP2012509830A (ja) 2008-11-24 2009-11-20 高cteガラスのレーザ援用フリット封着及び得られる封着ガラスパッケージ

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US12/276,631 US8245536B2 (en) 2008-11-24 2008-11-24 Laser assisted frit sealing of high CTE glasses and the resulting sealed glass package

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US8245536B2 (en) 2012-08-21
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JP2012509830A (ja) 2012-04-26
KR101530753B1 (ko) 2015-06-22
CN102264662A (zh) 2011-11-30
TW201033149A (en) 2010-09-16
EP2370372A1 (en) 2011-10-05
US20100129666A1 (en) 2010-05-27
TWI388526B (zh) 2013-03-11

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