WO2016108506A1 - Composition de getter contenant des particules d'oxyde de magnésium dopé avec un métal alcalin - Google Patents

Composition de getter contenant des particules d'oxyde de magnésium dopé avec un métal alcalin Download PDF

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Publication number
WO2016108506A1
WO2016108506A1 PCT/KR2015/014197 KR2015014197W WO2016108506A1 WO 2016108506 A1 WO2016108506 A1 WO 2016108506A1 KR 2015014197 W KR2015014197 W KR 2015014197W WO 2016108506 A1 WO2016108506 A1 WO 2016108506A1
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WO
WIPO (PCT)
Prior art keywords
getter
magnesium oxide
alkali metal
getter composition
doped
Prior art date
Application number
PCT/KR2015/014197
Other languages
English (en)
Korean (ko)
Inventor
변원배
김동환
이수희
박철희
Original Assignee
주식회사 엘지화학
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from KR1020150184054A external-priority patent/KR101834432B1/ko
Application filed by 주식회사 엘지화학 filed Critical 주식회사 엘지화학
Priority to CN201580058274.9A priority Critical patent/CN107073436A/zh
Priority to US15/510,200 priority patent/US20170297919A1/en
Publication of WO2016108506A1 publication Critical patent/WO2016108506A1/fr

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Classifications

    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K99/00—Subject matter not provided for in other groups of this subclass
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium

Definitions

  • Getter composition comprising magnesium oxide particles doped with alkali metal [recited citation with related application (s)]
  • the present invention relates to a getter composition comprising alkali metal doped oxide oxide particles, a getter layer comprising the same, and an organic electronic device including the same.
  • An organic electronic device refers to a device including an organic material layer that generates an exchange of electric charge using holes and electrons.
  • a photovoltaic device photovol tai c devi ce
  • Rectifiers rect ifi er
  • transmitters transmitters
  • organic light emitting diodes 0LEDs
  • an organic light emitting diode 0LED: Organi c Light Emitting Didoe
  • the 0LED is excellent in space utilization, and is expected to be applied in various fields including various portable devices, monitors, notebooks, and TVs.
  • the light emitting device which is an important device in the organic electronic device, has a disadvantage of being oxidized when it comes in contact with moisture
  • the sealing of the organic electronic device is important in the manufacturing process in order to improve durability and life of the organic electronic device. Accordingly, in order to effectively block the contact between the light emitting device and the moisture, water is blocked from two points of view, one is to block moisture by a physical seal, and the other is a material capable of absorbing moisture, that is, an organic electronic material. Device It is sealed together inside.
  • the physical sealing method is a method of connecting the front substrate and the back substrate with a highly adhesive sealing material so that the light emitting device is not exposed to the outside.
  • the moisture absorbent may be sealed together with the light emitting element to prevent the light emitting element from contacting with the moisture.
  • the composition containing a moisture absorber is called a getter composition.
  • an organic electronic device is manufactured by forming a light emitting device on a rear substrate and forming a getter layer on the front substrate using a getter composition to seal the front substrate and the back substrate.
  • the getter layer should use a material that not only has a high moisture absorption but also does not easily discharge absorbed moisture.
  • the getter layer should be transparent to transmit light emitted from the light emitting device.
  • a metal can or glass is processed in a cap form to have a groove, and a method of attaching a desiccant for absorbing moisture to the groove in powder form or preparing a film in form of a film and then using a double-sided tape to bond it.
  • the manner of mounting the first wet and dry process is complicated by the material and process cost increases, and "the thickness of the substrate whole thickening can not be used for the top emission is not a substrate for use in a transparent bag.
  • 10-2007-0072400 describes a method of incorporating a moisture absorbent into an epoxy sealant to chemically adsorb moisture introduced into an organic light emitting device to slow down the rate of penetration of water into the organic light emitting device. have.
  • the moisture adsorbent reacts with moisture to expand the volume, which may cause physical damage to the organic light emitting device.
  • the moisture adsorbent reacts with moisture to form a strong base material, such as a protective layer and a cathode layer. May cause chemical damage.
  • the conventional desiccant or desiccant is difficult to implement a transparent getter layer due to the large particle size, and thus it cannot be applied to a top-emiss type organic electronic device, such as a 0LED device, which can maximize luminous efficiency.
  • a top-emiss type organic electronic device such as a 0LED device
  • the durability and lifespan of the organic electronic device is lowered due to poor water absorption ability.
  • the present inventors studied the getter composition having excellent hygroscopicity and transparency, and as described below, the magnesium oxide particles doped with alkali metals significantly improved the degree of hygroscopicity compared to the magnesium oxide particles used in the prior art. It was.
  • the present invention relates to a method for producing a getter layer that can be formed uniformly on a substrate as well as having excellent hygroscopicity and transparency.
  • the present invention also relates to an organic electronic device comprising a getter layer produced by the above manufacturing method.
  • the present invention provides a getter composition comprising magnesium oxide particles doped with alkali metal.
  • the term 'getter composition' refers to a composition including a material capable of absorbing moisture, and a material absorbing moisture penetrated into a device including a moisture sensitive device such as an organic electronic device. Means.
  • a getter layer including the above-described getter composition having transparency and hygroscopicity is required.
  • a getter composition containing magnesium oxide particles is used come.
  • Magnesium oxide may be prepared from particles having a diameter of 100 nm or less, and in this case, not only has transparency but also may be usefully used for the getter layer due to the hygroscopicity of the magnesium oxide itself.
  • the magnesium oxide particles absorb about 10 ⁇ % of water by weight of magnesium oxide at the conditions of 60 ° C. and 40 Ritt, a material capable of further improving the water absorption is required. Therefore, in the present invention, magnesium oxide particles doped with alkali metals are used in place of the conventionally used magnesium oxide particles, and in this case, the amount of water absorption was remarkably increased.
  • the magnesium oxide particles doped with the alkali metal mean that the alkali metal is added to the crystal structure of the magnesium oxide particles. At this time, the addition amount of the alkali metal can be calculated as follows:
  • Doping amount (weight%) of alkali element (mass of alkali element (g)) / (MgO mass (g) + mass of alkali element (g)) X 100 Crystal structure of magnesium oxide particles, although not theoretically limited When alkali metal is added to the inside, defects are formed on the surface while replacing and invading lattice atoms, thereby increasing the surface area, and consequently, the amount of water absorption can be significantly increased.
  • the alkali metal is preferably Na, Li or K.
  • Doping amount of the alkali metal is 0.1 to 5 weight. A method of doping the alkali metal oxide particles will be described later.
  • the diameter of the magnesium oxide particles is preferably 5 to 50 nm.
  • the present invention is doped with the alkali metal comprising the following steps Provided are methods for preparing the oxide magnesium:
  • Step 1 is a step of mixing an alkali metal salt which is a precursor of magnesium oxide and an alkali metal to be doped.
  • the magnesium oxide may be commercially purchased and used, or may be prepared by the same method as the comparative example described later.
  • the alkali metal salt as the alkali metal salt
  • K 2 S0 4 or C3 ⁇ 4C00K can be used.
  • the doping amount of the alkali metal may be adjusted by adjusting the weight ratio of the magnesium oxide and the alkali metal salt, and it is preferable to mix an alkali metal salt of 0.1 to 5 weight 3 ⁇ 4 with respect to the magnesium oxide.
  • Step 2 is a step for removing the solvent from the reaction product of the mixture of step 1.
  • Mg (0H) 2 is produced, and the solvent of the mixture may be dried to obtain a product in powder form.
  • the drying is preferably carried out to the extent that the solvent can be sufficiently removed, for example, carried out at a temperature of 100 to 200 ° C, or vacuum drying Or lyophilization.
  • Step 3 is a step of preparing the magnesium oxide particles doped with alkali metal by heat treatment of the powder obtained in step 2. .
  • Magnesium oxide is formed in the heat treatment process, wherein the alkali metal present together participates in the formation of the magnesium oxide, and the alkali metal is doped in the crystal structure of the magnesium oxide.
  • the heat treatment is preferably performed at a temperature of 300 to 80CTC.
  • the heat treatment time is preferably heat-treated in a long time during the formation of magnesium oxide, for example, 30 minutes to 2 hours is preferable.
  • the heat treatment is preferably performed under an inert gas, and N 2 or Ar may be used as the inert gas.
  • N 2 or Ar may be used as the inert gas.
  • the present invention provides a getter layer comprising the getter composition as described above.
  • the getter layer includes the above-described alkali metal doped oxide oxide, and due to its transparency and hygroscopicity, the organic electrons It can be useful as a getter layer of a device.
  • the getter layer may further include a binder and the like to maintain the form of the getter layer and to improve adhesion to the substrate in contact with the getter layer.
  • the binder include polyvinylpyridone, citric acid, cellulose, acrylate polymers, polyurethanes, polyesters, and the like.
  • the method of using the getter composition as a getter layer of the organic electronic device is not particularly limited.
  • the getter layer may be formed by mixing the getter composition with an adsorbent solution and then applying or coating the entire surface of the substrate. have.
  • the coating method is not particularly limited, such as dip-coating, spin-coating, printing-coating and spray-coating methods.
  • the getter layer preferably has a thickness of 1 to 50. If it is less than 1, the degree of moisture absorption by the getter layer is small, and if it is more than 50i, the thickness of the getter layer becomes so thick that it is not suitable for miniaturization of the organic electronic device.
  • An example of the method used for the said getter layer all organic electronic device is shown in FIG. As shown in FIG.
  • the organic electroluminescent unit 12 is formed on the rear substrate 10, the getter layer 13 is formed on the front substrate 11, and then the organic electroluminescent unit 12 is formed.
  • the back substrate 10 and the front substrate 11 may be manufactured by sealing the sealing material 14 so that the getter layer 13 faces each other.
  • the organic electroluminescent unit 12 may be formed by evaporation, and may be formed in order of a crab 1 electrode, an organic film, and a crab 2 electrode.
  • the organic layer may include a hole injection layer, a hole transport layer, a light emitting layer, an electron injection layer, and / or an electron transport layer.
  • a glass substrate or a transparent plastic substrate may be used as the front substrate n, and when formed of a plastic substrate, an inner surface of the plastic substrate may further form a protective film for protecting from moisture.
  • the inner space partitioned by the front substrate 11 and the back substrate 10 is preferably maintained in a vacuum state or layered with an inert gas.
  • the present invention provides an organic electronic device including the getter layer. Examples of the organic electronic device include a photovoltaic device, a rectifier, a transmitter, and an organic light emitting diode (0LED).
  • the getter composition comprising magnesium oxide particles doped with alkali metals according to the present invention, while maintaining the transparency of the magnesium oxide particles used in the prior art, the degree of absorption is significantly improved, the getter layer comprising the same, and the getter layer Used in organic electronic devices, it is possible to effectively protect devices sensitive to moisture.
  • FIG 1 schematically shows the structure of an organic electronic device to which the getter layer of the present invention is applied.
  • Figure 2 shows the XRD analysis of the MgO prepared in Comparative Example of the present invention.
  • Figure 3 shows the results of XRD analysis of K-doped MgO prepared in Example 1 of the present invention.
  • Example 4 shows the results of XRD analysis of Li-doped MgO prepared in Example 2 of the present invention.
  • Figure 5 shows the moisture absorption test results of MgO, K-doped MgO and Li-doped MgO prepared in Comparative Examples, Examples 1 and 2 of the present invention.
  • Figure 6 shows the moisture absorption test results of Li-doped MgO and Na- doped MgO prepared in Examples 3 to 5 of the present invention.
  • Example 3 Preparation of Li -doped MgO Powder
  • Li-doped MgO powder was recovered. Doping amount of the Li is 1 weight 3 ⁇ 4, confirmed by ICP.
  • Example 5 Preparation of Na-doped MgO Powder
  • Example 1 Prepared in the same manner as in Example 1, using 0.086 g of NaN 3 instead of K 2 CO 3 , to recover the Na-doped MgO powder.
  • the Na doping amount is 1% by weight, and confirmed by ICP.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

La présente invention concerne une composition de getter contenant des particules d'oxyde de magnésium dopé avec un métal alcalin, une couche de getter contenant celle-ci, et un dispositif électronique organique comprenant la couche de getter. La composition de getter contenant les particules d'oxyde de magnésium dopé avec un métal alcalin, selon la présente invention, permet de maintenir la transparence des particules d'oxyde de magnésium existantes tout en améliorant significativement le pouvoir absorbant, ceci en faisant appel à la couche de getter contenant la composition de getter et en appliquant la couche de getter dans le dispositif électronique organique, les éléments sensibles à l'humidité pouvant ainsi être efficacement protégés.
PCT/KR2015/014197 2015-01-02 2015-12-23 Composition de getter contenant des particules d'oxyde de magnésium dopé avec un métal alcalin WO2016108506A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201580058274.9A CN107073436A (zh) 2015-01-02 2015-12-23 包含掺杂碱金属的氧化镁粒子的吸气剂组合物
US15/510,200 US20170297919A1 (en) 2015-01-02 2015-12-23 GETTER COMPOSITION COMPRISING MAGNESIUM OXIDE PARTICLES DOPED WITH ALKALI METAL (As Amended)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR10-2015-0000060 2015-01-02
KR20150000060 2015-01-02
KR1020150184054A KR101834432B1 (ko) 2015-01-02 2015-12-22 알칼리 금속이 도핑된 산화 마그네슘 입자를 포함하는 게터 조성물
KR10-2015-0184054 2015-12-22

Publications (1)

Publication Number Publication Date
WO2016108506A1 true WO2016108506A1 (fr) 2016-07-07

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WO (1) WO2016108506A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100088674A (ko) * 2007-10-04 2010-08-10 사에스 게터스 에스.페.아. 광전지 패널들을 제조하기 위한 혼합물 게터
KR20120021436A (ko) * 2010-07-30 2012-03-09 제일모직주식회사 흡습입자, 이를 포함하는 유기 ｅｌ 게터용 조성물 및 이를 이용한 유기 ｅｌ 소자
KR20120043027A (ko) * 2009-07-31 2012-05-03 제너럴 일렉트릭 캄파니 게터 물질을 갖는 밀폐형 패키지
KR20130019966A (ko) * 2011-08-18 2013-02-27 (주)엘지하우시스 수분 흡착제에 의해 감싸진 가스 흡착제를 포함하는 게터재 및 그 제조방법
KR20130074608A (ko) * 2011-12-26 2013-07-04 (주)엘지하우시스 고비표면적 게터재를 포함한 진공단열재

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100088674A (ko) * 2007-10-04 2010-08-10 사에스 게터스 에스.페.아. 광전지 패널들을 제조하기 위한 혼합물 게터
KR20120043027A (ko) * 2009-07-31 2012-05-03 제너럴 일렉트릭 캄파니 게터 물질을 갖는 밀폐형 패키지
KR20120021436A (ko) * 2010-07-30 2012-03-09 제일모직주식회사 흡습입자, 이를 포함하는 유기 ｅｌ 게터용 조성물 및 이를 이용한 유기 ｅｌ 소자
KR20130019966A (ko) * 2011-08-18 2013-02-27 (주)엘지하우시스 수분 흡착제에 의해 감싸진 가스 흡착제를 포함하는 게터재 및 그 제조방법
KR20130074608A (ko) * 2011-12-26 2013-07-04 (주)엘지하우시스 고비표면적 게터재를 포함한 진공단열재

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