US20080048178A1 - Tin phosphate barrier film, method, and apparatus - Google Patents

Tin phosphate barrier film, method, and apparatus Download PDF

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US20080048178A1
US20080048178A1 US11/509,445 US50944506A US2008048178A1 US 20080048178 A1 US20080048178 A1 US 20080048178A1 US 50944506 A US50944506 A US 50944506A US 2008048178 A1 US2008048178 A1 US 2008048178A1
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Prior art keywords
tin
phosphate
liquidus temperature
llt
tin phosphate
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US11/509,445
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English (en)
Inventor
Bruce Gardiner Aitken
Chong Pyung An
Benjamin Zain Hanson
Mark Alejandro Quesada
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Corning Inc
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Corning Inc
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Priority to US11/509,445 priority Critical patent/US20080048178A1/en
Assigned to CORNING INCORPORATED reassignment CORNING INCORPORATED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HANSON, BENJAMIN ZAIN, AITKEN, BRUCE GARDINER, AN, CHONG PYUNG, QUESADA, ALEJANDRO
Priority to EP07015335.8A priority patent/EP1892775B1/fr
Priority to EP15177347.0A priority patent/EP2955767B1/fr
Priority to JP2007212096A priority patent/JP4497482B2/ja
Priority to KR1020070084492A priority patent/KR100903245B1/ko
Priority to TW096131180A priority patent/TWI359518B/zh
Priority to CN2007101418005A priority patent/CN101130861B/zh
Publication of US20080048178A1 publication Critical patent/US20080048178A1/en
Priority to US12/553,469 priority patent/US7749811B2/en
Abandoned legal-status Critical Current

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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/80—Constructional details
    • H10K50/84—Passivation; Containers; Encapsulations
    • H10K50/844—Encapsulations
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/02—Details
    • H05B33/04—Sealing arrangements, e.g. against humidity
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
    • H01L31/042—PV modules or arrays of single PV cells
    • H01L31/048—Encapsulation of modules
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Definitions

  • the present invention relates to a method for inhibiting oxygen and moisture penetration, and the subsequent degradation of a device or apparatus.
  • the transport of oxygen or moisture through laminated or encapsulated materials and the subsequent attack of an inner material(s) represent two of the more common degradation mechanisms associated with many devices such as, for example, light-emitting devices (OLED devices), thin-film sensors, and evanescent waveguide sensors.
  • OLED devices light-emitting devices
  • thin-film sensors thin-film sensors
  • evanescent waveguide sensors evanescent waveguide sensors
  • the present invention provides a method of inhibiting oxygen and moisture penetration of a device, comprising the steps of: depositing a tin phosphate low liquidus temperature inorganic material on at least a portion of the device to create a deposited low liquidus temperature inorganic material; and heat treating the deposited low liquidus temperature inorganic material in a substantially oxygen and moisture free environment to form a hermetic seal; wherein the step of depositing the low liquidus temperature inorganic material comprises the use of a resistive heating element comprising tungsten.
  • the present invention provides a device produced by the methods of the present invention.
  • the present invention provides an organic electronic device comprising a substrate plate; at least one organic electronic or optoelectronic layer; and a tin phosphate low liquidus temperature barrier layer, wherein the electronic or optoelectronic layer is hermetically sealed between the tin phosphate low liquidus temperature barrier layer and the substrate plate.
  • the present invention provides an apparatus having at least a portion thereof sealed with a tin phosphate low liquidus temperature barrier layer.
  • FIG. 1 is a schematic illustration of an exemplary process of forming a tin phosphate LLT barrier layer on at least a portion of a device, in accordance with one aspect of the present invention.
  • FIG. 2 is a schematic of an exemplary device onto which a tin phosphate LLT barrier layer has been formed, in accordance with another aspect of the present invention.
  • FIG. 3 illustrates the steady, stable, high deposition rate achievable for a tin pyrophosphate LLT starting material when utilizing a tungsten boat, in accordance with one aspect of the present invention.
  • each of the combinations A-E, A-F, B-D, B-E, B-F, C-D, C-E, and C-F are specifically contemplated and should be considered disclosed from disclosure of A, B, and C; D, E, and F; and the example combination A-D.
  • any subset or combination of these is also specifically contemplated and disclosed.
  • the sub-group of A-E, B-F, and C-E are specifically contemplated and should be considered disclosed from disclosure of A, B, and C; D, E, and F; and the example combination A-D.
  • This concept applies to all aspects of this disclosure including, but not limited to, steps in methods of making and using the disclosed compositions.
  • steps in methods of making and using the disclosed compositions are if there are a variety of additional steps that can be performed it is understood that each of these additional steps can be performed with any specific embodiment or combination of embodiments of the disclosed methods, and that each such combination is specifically contemplated and should be considered disclosed.
  • Ranges can be expressed herein as from “about” one particular value, and/or to “about” another particular value. When such a range is expressed, another aspect includes from the one particular value and/or to the other particular value. Similarly, when values are expressed as approximations, by use of the antecedent “about,” it will be understood that the particular value forms another aspect. It will be further understood that the endpoints of each of the ranges are significant both in relation to the other endpoint, and independently of the other endpoint.
  • wt. % or “weight percent” or “percent by weight” of a component, unless specifically stated to the contrary, refers to the ratio of the weight of the component to the total weight of the composition in which the component is included, expressed as a percentage.
  • low liquidus temperature inorganic material refers to a material with a melting point (T m ) or glass transition temperature (T g ) less than about 1,000° C.
  • starting material refers to a material that will be evaporated and deposited onto a device.
  • a “deposited” material refers to a material that has been deposited on a device or apparatus.
  • a “barrier layer” refers to a hermetic coating, and specifically herein a deposited tin phosphate LLT material that has been heat treated to an temperature effective to form a hermetic seal.
  • the present invention provides an improved method for forming a tin phosphate LLT barrier layer on a device or apparatus.
  • the inventive method comprises the deposition of a tin phosphate LLT starting material onto at least a portion of a device or apparatus to form a deposited LLT material, and heat treatment of the deposited tin phosphate LLT material to remove defects and/or pores and form a tin phosphate LLT barrier layer.
  • the tin phosphate LLT material can be deposited onto the device by, for example, thermal evaporation, co-evaporation, laser ablation, flash evaporation, vapor-deposition, electron beam irradiation, or a combination thereof. Defects and/or pores in the tin phosphate LLT material can be removed by a consolidation or heat treatment step to produce a pore-free or substantially pore-free, oxygen and moisture impenetrable protective coating on the device. Although many deposition methods are possible with common glasses (i.e. those having high melting temperatures), the consolidation step is only practical with a tin phosphate LLT material where the consolidation temperature is sufficiently low so as to not damage the inner layers in the device. In some aspects, the deposition step and/or heat treatment step take place in a vacuum, in an inert atmosphere, or in ambient conditions depending upon the tin phosphate LLT material's composition.
  • FIG. 1 illustrates the steps of an exemplary method 100 for forming a tin phosphate LLT barrier layer on a device.
  • a device and a tin phosphate LLT starting material are provided so that one can form the desired tin phosphate LLT barrier layer on a device.
  • the tin phosphate LLT starting material is evaporated to deposit tin phosphate LLT material on at least a portion of the device.
  • the deposited tin phosphate LLT material can contain pores and can be remain permeable to oxygen and moisture.
  • the deposited tin phosphate LLT material is heat treated to a temperature sufficient to remove pores, for example, a temperature approximately equal to the glass transition temperature of the deposited tin phosphate LLT material, and form a hermetic seal or tin phosphate LLT barrier layer, which can prevent oxygen and moisture penetration into the device.
  • step 110 can be performed before, after, or simultaneous to step 120 .
  • the device of the present invention can be any such device where at least a portion of the device is sensitive to oxygen and/or moisture, for example, an organic-electronic device, such as an organic light emitting diode (“OLED”), a polymer light emitting diode (“PLED”), or a thin film transistor; a thin film sensor; an optoelectronic device, such as an optical switch or an evanescent waveguide sensor; a photovoltaic device; a food container; or a medicine container.
  • an organic-electronic device such as an organic light emitting diode (“OLED”), a polymer light emitting diode (“PLED”), or a thin film transistor
  • OLED organic light emitting diode
  • PLED polymer light emitting diode
  • a thin film transistor a thin film sensor
  • an optoelectronic device such as an optical switch or an evanescent waveguide sensor
  • a photovoltaic device such as a food container; or a medicine container.
  • the device is an OLED device that has multiple inner layers, including a cathode and an electro-luminescent material, which are located on a substrate.
  • the substrate can be any material suitable for fabricating and sealing a device.
  • the substrate is glass.
  • the substrate can be a flexible material.
  • the LLT material is deposited prior to the deposition of an organic electro-luminescent material.
  • the device is an organic electronic device comprising a substrate, as described above, and at least one organic electronic or optoelectronic layer.
  • the device is coated with a tin phosphate LLT barrier layer, wherein the organic electronic or optoelectronic layer is hermetically sealed between the substrate and the tin phosphate LLT barrier layer.
  • the hermetic seal is created by the deposition and heat treatment of a tin phosphate LLT material.
  • At least a portion of the device is sealed with a tin phosphate LLT material, wherein the tin phosphate LLT material comprises tin phosphate material.
  • FIG. 2 depicts an exemplary cross-sectional side view of a device coated with a tin phosphate LLT barrier layer.
  • the exemplary coated device 10 of FIG. 2 includes a substrate 40 , an optoelectronic layer 20 that is sensitive to oxygen and/or moisture, and a tin phosphate LLT barrier layer 30 that provides a hermetic seal between the optoelectronic layer 20 and environmental oxygen and moisture.
  • the physical properties, such as low glass transition temperature, of a low liquidus temperature inorganic material facilitate the formation of a hermetic seal.
  • a tin phosphate low liquidus temperature inorganic starting material, or LLT starting material can be deposited onto a least a portion of a device and the deposited material heat treated at a relatively low temperature to obtain a pore-free or substantially pore-free barrier layer, without thermally damaging the device's inner layer(s). It should be appreciated that the deposited and heat treated low liquidus temperature inorganic material can be used as a barrier layer on a wide variety of devices.
  • the tin phosphate LLT starting material has a glass transition temperature of less than about 1000° C., preferably less than about 600° C., and more preferably less than about 400° C.
  • the tin phosphate LLT starting material is substantially free of fluorine, preferably containing less than one weight percent fluorine, and more preferably being free of fluorine.
  • the tin phosphate LLT starting material comprises tin, phosphorus, and oxygen.
  • Exemplary tin phosphate LLT starting materials include, tin meta-phosphate, tin ortho-hydrogenphosphate, tin ortho-dihydrogenphosphate, tin pyrophosphate, or a mixture thereof. It is preferred that the tin phosphate LLT starting material be a tin pyrophosphate.
  • the stoichiometry of the deposited tin phosphate LLT material can vary from that of the tin phosphate LLT starting material.
  • evaporation of a tin pyrophosphate can produce a deposited material that is depleted or enriched in phosphorus relative to tin pyrophosphate.
  • the deposited tin phosphate LLT material can have a tin concentration that is lower than, equal to, or higher than that of the tin phosphate LLT starting material. It can be advantageous if the deposited tin phosphate LLT material has a tin concentration higher than that of the tin phosphate LLT starting material.
  • the deposited tin phosphate LLT material have a tin concentration at least as high as that of the tin phosphate LLT starting material. It is also preferable that the deposited tin phosphate LLT material have substantially the same low liquidus temperature as the tin phosphate LLT starting material. It is also preferable that the tin phosphate LLT starting material comprise divalent tin.
  • the tin phosphate LLT starting material of the present invention can be crystalline, amorphous, glassy, or a mixture thereof.
  • the tin phosphate LLT starting material can comprise at least one crystalline component.
  • the tin phosphate LLT starting material can comprise at least one amorphous component.
  • the LLT starting material can comprise at least one glassy component.
  • the tin phosphate LLT starting material is a single tin phosphate LLT material such as, for example, tin meta-phosphate, tin ortho-hydrogen phosphate, tin ortho-dihydrogen phosphate, or tin pyrophosphate.
  • the tin phosphate LLT starting material can comprise a mixture of components.
  • the tin phosphate LLT starting material can comprise a glass, formed by mixing at least two tin phosphate LLT materials, heating the materials to fuse them together, and quenching the resulting mixture to form a glass.
  • the tin phosphate LLT starting material can further comprise a tin oxide.
  • the tin oxide material can comprise from about 60 to about 85 mole percent of the tin phosphate LLT starting material.
  • the tin phosphate LLT starting material can further comprise additives and/or other low liquidus temperature materials.
  • the tin phosphate LLT starting material comprises a niobium containing compound.
  • the tin phosphate LLT starting material comprises niobium oxide, at an amount from greater than 0 to about 10 weight percent, preferably at an amount from greater than 0 to about 5 weight percent, and more preferably at about 1 weight percent.
  • Tin phosphate LLT starting materials are commercially available, for example, from Alfa Aesar, Ward Hill, Mass., USA. One of ordinary skill in the art should be able to readily select an appropriate tin phosphate starting material.
  • the tin phosphate LLT starting material can be deposited onto at least a portion of a device by an evaporative process, such as thermal evaporation.
  • the evaporation and deposition steps of the present invention are not limited to any specific equipment or geometric arrangement. It should be noted that the evaporation and deposition steps can be referred to a separate steps or as a combined step.
  • the evaporated material will typically deposit on surfaces proximally located to the resistive heating element.
  • Commonly used evaporation systems operate under vacuum at pressures, for example, from about 10 ⁇ 8 to about 10 ⁇ 5 Torr and are fitted with leads to provide electrical current to a resistive heating element.
  • Evaporation can also be performed in an inert atmosphere to ensure substantially oxygen and moisture free conditions are maintained throughout the evaporation, deposition, and sealing process. Unless required by the nature of the device to be coated, it is not necessary that the deposition and/or heat treatment environment be completely free of oxygen and moisture, and so, the environment can be free of or substantially free of oxygen and moisture.
  • a variety of resistive heating elements can be employed, including boats, ribbons, or crucibles.
  • the tin phosphate LLT starting material can be placed in contact with the resistive heating element. Current, typically in the range of 80 to 180 Watts, is subsequently passed through the resistive heating element, resulting in volatilization of the tin phosphate LLT starting material.
  • the power required to evaporate a specific material will vary, depending on the material itself, the pressure, and the resistance of the heating element.
  • the rate and length of time of a specific deposition will vary, depending upon the materials, deposition conditions, and the desired thickness of the deposited layer.
  • Evaporation systems are commercially available, for example, from Kurt J. Lesker Company, Clairton, Pa., USA.
  • Kurt J. Lesker Company Clairton, Pa., USA.
  • One of ordinary skill in the art could readily select an evaporation system and the operating conditions necessary to deposit a tin phosphate LLT material.
  • a single layer of a tin phosphate LLT material can be deposited on at least a portion of a substrate.
  • multiple layers of the same or varying types of tin phosphate LLT material can be deposited over one or more inner layers, positioned on top of a substrate.
  • the present invention comprises a resistive heating element comprised of tungsten.
  • the geometry of the evaporative system and of the resistive heating element can vary.
  • the resistive tungsten heating element is a boat.
  • the resistive tungsten heating element is a ribbon.
  • One of ordinary skill in the art should readily be able to select an appropriate evaporative system and resisting tungsten heating element.
  • Evaporation of a tin phosphate LLT starting material from a resistive tungsten heating element provides high, steady state, deposition rates that are difficult to achieve with other LLT starting materials or deposition techniques. For example, a deposition rate as high as 15 ⁇ per second is attainable using a tin pyrophosphate LLT starting material and a small tungsten boat.
  • the ability to deposit tin phosphate LLT starting materials at such rates makes feasible the commercial fabrication of flexible substrates that are able to withstand high processing temperatures.
  • the deposited tin phosphate LLT material can optionally further comprise a tin oxide.
  • the deposited tin phosphate LLT material can comprise from about 60 to about 85 mole percent tin oxide.
  • the specific chemical structure and stoichiometry of the deposited tin phosphate LLT material can vary from that of the tin phosphate LLT starting material.
  • the presence of tin oxide in the deposited tin phosphate LLT material can result from the optional addition of a tin oxide material to the tin phosphate LLT starting material, or from chemical and/or stoichiometric changes occurring during the deposition process or on the surface of the device.
  • the deposited tin phosphate LLT material comprises divalent tin, a higher valence tin compound, for example, a Sn +4 compound, or a mixture of thereof.
  • a Sn +4 compound for example, a Sn +4 compound, or a mixture of thereof.
  • the presence of a Sn +4 compound in the deposited LLT material provides enhanced durability.
  • Evaporation of a tin phosphate LLT starting material using a resistive tungsten heating element can lead to a chemical or physical reaction between the tin phosphate LLT starting material and the resistive tungsten heating element, wherein at least a portion of the tungsten can be deposited together with the tin phosphate LLT starting material.
  • the deposited tin phosphate LLT material comprises from greater than 0 to about 10 weight percent tungsten, preferably from about 2 to about 7 weight percent tungsten.
  • a reaction between a tin phosphate LLT starting material, such as for example, tin pyrophosphate, and a tungsten heating element results in the formation of a green glassy material which comprises tungsten.
  • the deposited tin phosphate LLT material can contain other materials to provide improved strength or resistance to permeability, or to alter the optical properties of the device. These materials can be evaporated together with the tin phosphate LLT starting material.
  • the deposited tin phosphate LLT material can contain niobium, for example, in the form of niobium oxide. Niobium oxide is commercially available from Alfa Aesar, Ward Hill, Massachusetts, USA. One of ordinary skill in the art could readily select an appropriate additional material, such as a niobium oxide.
  • the deposited tin phosphate LLT material comprises a tin phosphate, niobium, and tungsten.
  • a heat treatment or annealing step minimizes defects and pores in the deposited layer of tin phosphate LLT material, allowing the formation of a hermetic seal or tin phosphate LLT barrier layer.
  • the heat treated tin phosphate LLT barrier layer is pore-free or substantially pore-free.
  • the number and/or size of pores remaining in the heat treated tin phosphate LLT barrier layer should be sufficiently low to prevent oxygen and moisture penetration.
  • the heat treatment is performed under vacuum.
  • the heat treatment step is performed in an inert atmosphere. It should be appreciated that the heat treatment step can be performed in the same system and immediately subsequent to the deposition step, or at a separate time and place provided that environmental conditions are maintained to prevent oxygen and moisture intrusion into the device.
  • the heat treatment step of the present invention comprises heating the device onto which a tin phosphate LLT material has been deposited.
  • the temperature to which the device and deposited tin phosphate LLT material are exposed is approximately equal to the glass transition temperature, or T g , of the deposited tin phosphate LLT material.
  • the temperature to which the device and deposited tin phosphate LLT material are exposed is within approximately 50° C. of the glass transition temperature, or T g , of the deposited tin phosphate LLT material.
  • the temperature to which the device and deposited tin phosphate LLT material are exposed is from about 200° C.
  • the temperature to which the device and deposited tin phosphate LLT material are exposed is from about 250° C. to about 270° C. It will be appreciated that the ideal time and temperature to which a device and deposited tin phosphate LLT material are exposed will vary, depending on factors such as the composition of the deposited tin phosphate LLT material, the working temperature range of the components to be sealed, and the desired thickness and permeability of the hermetic seal.
  • the heat treatment step can be performed by any heating means that can achieve the desired temperature and maintain a substantially oxygen and moisture free environment.
  • the heat treatment step comprises heating the device with an infrared lamp positioned in the vacuum deposition chamber. In another aspect, the heat treatment step comprises raising the temperature of the vacuum deposition chamber in which the device is located.
  • the heat treatment step can be performed separately from the deposition step, provided that a substantially oxygen and moisture free environment is maintained. It is preferable that the heat treatment conditions be sufficient to allow the resulting device to meet desired performance criteria, such as the calcium patch test described below.
  • desired performance criteria such as the calcium patch test described below.
  • the thickness of the tin phosphate LLT barrier layer can be any such thickness required to provide the desired hermetic seal.
  • the tin phosphate LLT barrier layer is about 1 micrometer thick. In another aspect, the tin phosphate LLT barrier is about 2.5 micrometers thick.
  • the tin phosphate LLT barrier layer is at least partially transparent to radiation either emitted by or absorbed by the device. In another aspect, the tin phosphate LLT barrier layer is at least partially transparent to visible light.
  • the hermeticity of a tin phosphate LLT barrier layer can be evaluated using various methods to test the hermeticity of the tin phosphate LLT barrier layer to oxygen and/or moisture.
  • the tin phosphate LLT barrier layer can be evaluated using a calcium patch test, wherein a thin calcium film is deposited onto a substrate. A tin phosphate LLT barrier layer is then formed, sealing the calcium film between the tin phosphate LLT barrier layer and the substrate. The resulting device is then subjected to environmental aging at a selected temperature and humidity, for example, 85° C. and 85% relative humidity.
  • a tin pyrophosphate LLT material was deposited onto a silicon wafer by thermal evaporation.
  • Pellets of tin pyrophosphate (Alfa Aesar, Ward Hill, Mass., USA) were prepared with a home-made pill press and stored in a 100° C. oven.
  • the tin pyrophosphate pellets were placed in a 3 inch by 0.75 inch tungsten boat (S7-.010W, available from R.D. Mathis, Long Beach, Calif., USA), clamped between the two copper leads of an evaporative system.
  • the vacuum chamber of the evaporator system was evacuated to an ultimate pressure of between 10 ⁇ 6 and 10 ⁇ 5 Torr, and the silicon wafer positioned out of the evaporation plume path.
  • the power was adjusted to approximately 20 Watts and held for approximately 30 minutes to allow the tin pyrophosphate and tungsten boat to react. When current was applied, stable deposition rates as high as 15 ⁇ per second were achieved.
  • a tin pyrophosphate LLT material was deposited onto a calcium patch test device. Pellets of tin pyrophosphate were prepared and evaporated as in Example 1. The power was adjusted to 20 Watts and held for 30 minutes to allow the tin pyrophosphate and tungsten boat to react. Power was then increased to deliver 80 to 125 Watts to the tungsten boat.
  • a residual gas analyzer monitored the vacuum chamber environment. As depicted in FIG. 3 , a relatively low concentration of background gasses was present during evaporation. After an initial period, the power was adjusted to achieve a stable deposition rate of between 10 and 15 ⁇ per second, at which time the test device was positioned in the evaporation plume path to deposit the LLT material.
  • a calcium patch test device as in Example 2, was prepared and sealed with a LLT material.
  • one mole percent of niobium pentoxide was added to the starting tin pyrophosphate material, prior to evaporation. Similar deposition rates to those of Example 2 were achieved.
  • the test device was then subjected to an accelerated aging test as described in Example 6, the results of which are detailed in Table 1.
  • a calcium patch test device was prepared.
  • the test device consisted of a Corning 1737 glass substrate (approximately 1 millimeter thick and 2.5 inches square), onto which a 100 nanometer thick calcium film (approximately 1 inch by 0.5 inch) was deposited, and onto which a 200 nanometer thick aluminum layer (approximately 1 inch by 0.5 inch) was deposited.
  • the test device was affixed to moveable platform in the vacuum deposition chamber.
  • the calcium patch test device was subsequently sealed with a deposited tin pyrophosphate LLT material.
  • the sealed device was then exposed to conditions designed to mimic long term operation of a device, such as an OLED.
  • Industry standard conditions for accelerated aging require a device to withstand 1000 hours in an 85° C. and 85% relative humidity environment.
  • moisture or oxygen by permeation through the LLT layer, the calcium reacts and changes from a highly reflective film to an opaque white crust.
  • Optical photographs were acquired at regular time intervals to quantify the evolution of the test device and thus, determine the hermetic strength of the LLT layer.
  • Table 1 below details calcium patch experiments on devices prepared as in examples above. The samples detailed in Table 1 are not necessarily the specific samples prepared in Examples 1-4, but were prepared in the same manner.
  • Table 1 illustrates that barrier layers formed from the evaporation of tin pyrophosphate using a tungsten heating element yielded good hermetic seals when heat treated to temperatures near the glass transition temperature of the LLT material for a period of 2 hours.
  • An additional film was prepared according to Example 3, wherein the tin phosphate LLT starting material included 1 mole percent niobium pentoxide.
  • Table 1 illustrates the ability to achieve good hermetic seals using a tin phosphate LLT material when a deposited film is heat treated to a temperature near the glass transition temperature of the LLT material.

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US11/509,445 2006-08-24 2006-08-24 Tin phosphate barrier film, method, and apparatus Abandoned US20080048178A1 (en)

Priority Applications (8)

Application Number Priority Date Filing Date Title
US11/509,445 US20080048178A1 (en) 2006-08-24 2006-08-24 Tin phosphate barrier film, method, and apparatus
EP07015335.8A EP1892775B1 (fr) 2006-08-24 2007-08-04 Film barrière au phosphate d'étain et procédé
EP15177347.0A EP2955767B1 (fr) 2006-08-24 2007-08-04 Film barrière au phosphate d'étain, procédé et appareil
JP2007212096A JP4497482B2 (ja) 2006-08-24 2007-08-16 デバイスへの酸素および水分の浸透を防ぐ方法
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TW200830597A (en) 2008-07-16
EP1892775A3 (fr) 2009-11-25
CN101130861A (zh) 2008-02-27
CN101130861B (zh) 2010-11-03
US20090324830A1 (en) 2009-12-31
EP2955767B1 (fr) 2019-03-06
TWI359518B (en) 2012-03-01
KR100903245B1 (ko) 2009-06-17
JP4497482B2 (ja) 2010-07-07
EP1892775A2 (fr) 2008-02-27
US7749811B2 (en) 2010-07-06
JP2008053715A (ja) 2008-03-06
KR20080018817A (ko) 2008-02-28
EP2955767A1 (fr) 2015-12-16
EP1892775B1 (fr) 2015-10-07

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