GETTER COMPOSITION COMPRISING MAGNESIUM OXIDE PARTICLES DOPED WITH ALKALI METAL (As Amended)

20170297919 · 2017-10-19

    Inventors

    Cpc classification

    International classification

    Abstract

    The present invention relates to a getter composition comprising magnesium oxide particle doped with alkali metal, a getter layer comprising the same, and an organic electronic device comprising the getter layer. The getter composition comprising magnesium oxide particle doped with alkali metal according to the present invention has remarkably improved hygroscopicity simultaneously with maintaining transparency of the previously used magnesium oxide particles, and thus, is used in a getter layer comprising the same and an organic electronic device comprising the getter layer, thereby effectively protecting water sensitive devices.

    Claims

    1. A getter composition comprising magnesium oxide particles doped with alkali metal.

    2. The getter composition according to claim 1, wherein the alkali metal is Na, Li, or K.

    3. The getter composition according to claim 1, wherein the magnesium oxide particles have a diameter of 5 to 50 nm.

    4. The getter composition according to claim 1, wherein the magnesium oxide particles doped with alkali metal are prepared by a method comprising the step of: 1) mixing magnesium oxide and alkali metal salt to prepare a mixture; 2) drying the mixture; and 3) heat-treating the dried mixture.

    5. The getter composition according to claim 4, wherein the alkali metal salt is NaN.sub.3, NaCO.sub.3, NaOH, NaCl, NaNO.sub.3, Na.sub.2SO.sub.4, CH.sub.3COONa, LiN.sub.3, Li.sub.2CO.sub.3, LiOH, LiCl, LiNO.sub.3, Li.sub.2SO.sub.4, CH.sub.3COOLi, KN.sub.3, K.sub.2CO.sub.3, KOH, KCl, KNO.sub.3, K.sub.2SO.sub.4, or CH.sub.3COOK.

    6. The getter composition according to claim 4, wherein, based on the magnesium oxide, 0.1 to 5 wt % of alkali metal salt is mixed.

    7. The getter composition according to claim 4, wherein the solvent of the mixture is water, etyleneglycol, methanol, or ethanol.

    8. The getter composition according to claim 4, wherein the drying is carried out at a temperature of 100 to 200° C., or by vacuum drying or freeze drying.

    9. The getter composition according to claim 4, wherein the heat-treatment is carried out at a temperature of 300 to 800° C.

    10. The getter composition according to claim 4, wherein the heat-treatment is carried out for 30 minutes to 2 hours.

    11. A getter layer comprising the getter composition according to claim 1.

    12. The getter layer according to claim 11, wherein the thickness of the getter layer is 1 to 50 um.

    13. An organic electronic device comprising the getter layer of claim 11.

    Description

    BRIEF DESCRIPTION OF THE DRAWINGS

    [0049] FIG. 1 schematically shows the structure of an organic electronic device for which the getter layer of the present invention is applied.

    [0050] FIG. 2 shows the XRD analysis result of MgO prepared in Comparative Example.

    [0051] FIG. 3 shows the XRD analysis result of K-doped MgO prepared in Example 1 of the present invention.

    [0052] FIG. 4 shows the XRD analysis result of Li-doped MgO prepared in Example 2 of the present invention.

    [0053] FIG. 5 shows the hygroscopicity test results of MgO, K-doped MgO and Li-doped MgO prepared in Comparative Example, Examples 1 and 2 of the present invention.

    [0054] FIG. 6 shows the hygroscopicity test results of Li-doped MgO and Na-doped MgO prepared in Examples 3 to 5 of the present invention.

    DETAILED DESCRIPTION OF THE EMBODIMENTS

    [0055] Hereinafter, preferable examples are presented for better understanding of the present invention. However, these examples are provided only to more easily understand the present invention, and the scope of the present invention is not limited thereto.

    Comparative Example: Preparation of MgO Powder

    [0056] 51.3 g of Mg(NO.sub.3).sub.2-6H.sub.2O was dissolved in 75 mL of distilled water, and 25 mL of ethylene glycol was added thereto. 16 g of NaOH was dissolved in 30 mL of water, which was added to the above solution to precipitate Mg(OH).sub.2. The precipitate was washed with distilled water and ethanol sequentially, and sufficiently dried at 150° C. to obtain powder. The obtained powder was heat-treated under nitrogen atmosphere at 400° C. for 1 hour to obtain MgO powder.

    Example 1: Preparation of K-Doped MgO Powder

    [0057] 3 g of MgO prepared in Comparative Example was introduced into 20 mL of distilled water, a solution of 0.054 g of K.sub.2CO.sub.3 dissolved in 20 mL of distilled water was introduced therein, and the mixed solution was stirred. The solution was sufficiently dried at 150° C. to obtain powder. The obtained powder was heat-treated under nitrogen atmosphere at 400° C. for 1 hour to obtain K-doped MgO powder. The doped amount of K was 1 wt %, which was confirmed by ICP (Inductively Coupled Plasma).

    Example 2: Preparation of Li-Doped MgO Powder

    [0058] Li-doped MgO powder was obtained by the same method as Example 1, except using 0.161 g of Li.sub.2CO.sub.3 instead of K.sub.2CO.sub.3. The doped amount of Li was 1 wt %, which was confirmed by ICP.

    Example 3: Preparation of Li-Doped MgO Powder

    [0059] Li-doped MgO powder was obtained by the same method as Example 1, except using 0.183 g of LiOH—H.sub.2O instead of K.sub.2CO.sub.3. The doped amount of Li was 1 wt %, which w as confirmed by ICP.

    Example 4: Preparation of Li-Doped MgO Powder

    [0060] Li-doped MgO powder was obtained by the same method as Example 1, except using 0.301 g of LiNO.sub.3 instead of K.sub.2CO.sub.3. The doped amount of Li was 1 wt %, which was confirmed by ICP.

    Example 5: Preparation of Na-Doped MgO Powder

    [0061] Na-doped MgO powder was obtained by the same method as Example 1, except using 0.086 g of NaN.sub.3 instead of K.sub.2CO.sub.3. The doped amount of Na was 1 wt %, which was confirmed by ICP.

    Experimental Example 1: XRD Result

    [0062] In order to confirm MgO crystallinities of MgO powder and K-doped MgO powder respectively prepared in Comparative Example and Examples 1 and 2, XRD analysis was conducted, and the results are shown in FIGS. 2 to 4.

    [0063] As shown in FIGS. 2 and 3, it was confirmed that the XRS pattern of MgO of Comparative Example in FIG. 2 almost correspond with the XRD pattern of K-doped MgO of Example 1 in FIG. 3. It was also confirmed that the XRD pattern of Li-doped MgO of Example 2 in FIG. 4 almost correspond with the XRD pattern of MgO of Comparative Example in FIG. 2.

    [0064] From the foregoing results, it was confirmed that even in case MgO is doped with alkali metal, the crystallinity of MgO is maintained intact.

    Experimental Example 2: Hygroscopicity Test

    [0065] 0.3 to 0.5 g of the powder prepared in Comparative Example and Examples 1 to 5 were respectively put in a vial, and it was put in a thermo-hygrostat (60° C., 40 RH %), and then, mass was measured at fixed times, thus measuring moisture absorption amount.

    [0066] The test results are shown in FIG. 5 and FIG. 6. As shown in FIG. 5 and FIG. 6, hygroscopicity remarkably increased compared to MgO of Comparative Example, and particularly, in the case of Example 1, moisture absorption amount remarkably increased by about 2.5 times.

    DESCRIPTION OF SYMBOLS

    [0067] 10: rear substrate [0068] 11: front substrate [0069] 12: organic electroluminescence part [0070] 13: getter layer [0071] 14: sealant