US2024410055A1PendingUtilityA1

Method and formulation for preparing optical metal oxide layers

Assignee: MERCK PATENT GMBHPriority: Oct 8, 2021Filed: Oct 4, 2022Published: Dec 12, 2024
Est. expiryOct 8, 2041(~15.2 yrs left)· nominal 20-yr term from priority
C23C 18/1291C23C 18/06C23C 18/04C23C 18/143C23C 18/1225C23C 18/1245C23C 18/1295C23C 18/1216
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Claims

Abstract

The present invention relates to a method for preparing an optical metal oxide layer, to a formulation for preparing an optical metal oxide layer and to an optical device comprising an optical metal oxide layer. The optical metal oxide layers are particularly suitable for optical applications and may be used in optical devices such as, for example, in diffractive gratings for augmented reality (AR) and/or virtual reality (VR) devices.

Claims

exact text as granted — not AI-modified
1 . Method for preparing an optical metal oxide layer comprising the following steps:
 (a) providing a formulation comprising one or more titanium polyoxometalates (POMs) and one or more formulation media;   (b) applying the formulation to a surface of a substrate; and   (c) converting the formulation on the surface of the substrate to an optical metal oxide layer.   
     
     
         2 . Method according to  claim 1 , wherein the one or more titanium polyoxometalates (POMs) comprise independently from each other three or more titanium atoms and one or more ligand species. 
     
     
         3 . Method according to  claim 1 , wherein the titanium polyoxometalates (POMs) are independently from each other represented by the following Formula (1): 
       
         
           
             
               
                 
                   
                     
                       { 
                       
                         
                           
                             
                               Ti 
                               u 
                             
                             ( 
                             
                               
                                 μ 
                                 2 
                               
                               - 
                               OH 
                             
                             ) 
                           
                           v 
                         
                         ⁢ 
                         
                           
                             ( 
                             
                               
                                 μ 
                                 3 
                               
                               - 
                               OH 
                             
                             ) 
                           
                           w 
                         
                         ⁢ 
                         
                           
                             ( 
                             
                               
                                 μ 
                                 2 
                               
                               - 
                               O 
                             
                             ) 
                           
                           x 
                         
                         ⁢ 
                         
                           
                             ( 
                             
                               
                                 μ 
                                 3 
                               
                               - 
                               O 
                             
                             ) 
                           
                           y 
                         
                         ⁢ 
                         
                           
                             ( 
                             
                               
                                 μ 
                                 4 
                               
                               - 
                               O 
                             
                             ) 
                           
                           z 
                         
                       
                       } 
                     
                     ⁢ 
                     
                       
                         ∏ 
                         
                           j 
                           = 
                           1 
                         
                         
                           j 
                           = 
                           n 
                         
                       
                         
                       
                         
                           ( 
                           
                             L 
                             j 
                           
                           ) 
                         
                         
                           a 
                           j 
                         
                       
                     
                   
                 
                 
                   
                     Formula 
                     ⁢ 
                         
                     
                       ( 
                       1 
                       ) 
                     
                   
                 
               
             
           
         
       
       wherein:
 μ 2 -OH represents a bidentate bridging hydroxo; 
 μ 3 -OH represents a tridentate bridging hydroxo; 
 μ 2 -O represents a bidentate bridging oxido; 
 μ 3 -O represents a tridentate bridging oxido; 
 μ 4 -O represents a tetradentate bridging oxido; 
 L j  represents at each occurrence independently from each other a ligand species; 
 a j  is at each occurrence independently from each other an integer from 1 to 100; 
 n is an integer from 2 to 10; 
 u is an integer from 2 to 100; 
 v is an integer from 0 to 100; 
 w is an integer from 0 to 100; 
 x is an integer from 0 to 100; 
 y is an integer from 0 to 100; and 
 z is an integer from 0 to 100. 
 
     
     
         4 . Method according to  claim 3 , wherein the following equation is fulfilled: 
       
         
           
             
               
                 
                   
                     4 
                     * 
                   
                   ⁢ 
                   u 
                 
                 - 
                 
                   [ 
                   
                     v 
                     + 
                     w 
                     + 
                     
                       
                         2 
                         * 
                       
                       ⁢ 
                       
                         ( 
                         
                           x 
                           + 
                           y 
                           + 
                           z 
                         
                         ) 
                       
                     
                     + 
                     
                       
                         ∑ 
                         
                           j 
                           = 
                           1 
                         
                         
                           j 
                           = 
                           n 
                         
                       
                         
                       
                         ( 
                         
                           
                             
                               
                                 m 
                                 j 
                               
                               ( 
                               
                                 L 
                                 j 
                               
                               ) 
                             
                             * 
                           
                           ⁢ 
                           
                             a 
                             j 
                           
                         
                         ) 
                       
                     
                   
                   ] 
                 
               
               = 
               c 
             
           
         
         wherein: 
         m j (L j ) represents the amount of negative charge of L j ; and 
         c represents the total charge of the titanium polyoxometalate (POM); 
         and a j , n, u, v, w, x, y and z are defined as in  claim 3 . 
       
     
     
         5 . Method according to  claim 1 , wherein the one or more titanium polyoxometalates (POMs) are independently from each other selected from Ti 12  polyoxometalates, Tins polyoxometalates, Ti 18  polyoxometalates, Ti 44  polyoxometalates, and Ti 52  polyoxometalates. 
     
     
         6 . Method according to  claim 1 , wherein the mass ratio of titanium polyoxometalates (POMs) in the formulation is in the range from 0.1% to 50% (w/w) based on the total mass of the formulation. 
     
     
         7 . Method according to  claim 1 , wherein the formulation provided in step (a) further comprises one or more additives selected from surfactants, wetting and dispersion agents, adhesion promoters, and polymer matrices. 
     
     
         8 . Method according to  claim 1 , wherein the formulation is applied in step (b) to a surface of a substrate by a deposition method, preferably by a drop casting method, a coating method, or a printing method. 
     
     
         9 . Method according to  claim 1 , wherein step (b) is carried out several times in succession. 
     
     
         10 . Method according to  claim 1 , wherein in step (c) the formulation is converted on the surface of the substrate to an optical metal oxide layer by exposure to thermal treatment and/or irradiation treatment. 
     
     
         11 . Method according to  claim 1 , wherein in step (c) the formulation is converted on the surface of the substrate to an optical metal oxide layer by pre-baking at a temperature from 40 to 150° C.; and then baking at a temperature from 150 to 600° C. 
     
     
         12 . Method according to  claim 1 , wherein the substrate is a patterned substrate comprising topographical features on the surface thereof. 
     
     
         13 . Method according to  claim 12 , wherein the optical metal oxide layer covers the surface of the substrate and fills said topographical features. 
     
     
         14 . Method according to  claim 12 , wherein the topographical features have an aspect ratio of 1:20 to 20:1. 
     
     
         15 . Formulation for preparing an optical metal oxide layer, wherein the formulation comprises:
 (i) one or more titanium polyoxometalates (POMs);   (ii) one or more formulation media; and   (iii) one or more additives selected from surfactants, wetting and dispersion agents, adhesion promoters, and polymer matrices.   
     
     
         16 . Formulation according to  claim 15 , wherein the titanium polyoxometalates (POMs) comprise independently from each other three or more titanium atoms and one or more ligand species. 
     
     
         17 . Formulation according to  claim 15 , wherein the titanium polyoxometalates (POMs) are independently from each other represented by the following Formula (1): 
       
         
           
             
               
                 { 
                 
                   
                     
                       
                         Ti 
                         u 
                       
                       ( 
                       
                         
                           μ 
                           2 
                         
                         - 
                         OH 
                       
                       ) 
                     
                     v 
                   
                   ⁢ 
                   
                     
                       ( 
                       
                         
                           μ 
                           3 
                         
                         - 
                         OH 
                       
                       ) 
                     
                     w 
                   
                   ⁢ 
                   
                     
                       ( 
                       
                         
                           μ 
                           2 
                         
                         - 
                         O 
                       
                       ) 
                     
                     x 
                   
                   ⁢ 
                   
                     
                       ( 
                       
                         
                           μ 
                           3 
                         
                         - 
                         O 
                       
                       ) 
                     
                     y 
                   
                   ⁢ 
                   
                     
                       ( 
                       
                         
                           μ 
                           4 
                         
                         - 
                         O 
                       
                       ) 
                     
                     z 
                   
                 
                 } 
               
               ⁢ 
               
                 
                   ∏ 
                   
                     j 
                     = 
                     1 
                   
                   
                     j 
                     = 
                     n 
                   
                 
                   
                 
                   
                     ( 
                     
                       L 
                       j 
                     
                     ) 
                   
                   
                     a 
                     j 
                   
                 
               
             
           
         
         Formula (1) 
       
       wherein:
 μ 2 -OH represents a bidentate bridging hydroxo; 
 μ 3 -OH represents a tridentate bridging hydroxo; 
 μ 2 -O represents a bidentate bridging oxido; 
 μ 3 -O represents a tridentate bridging oxido; 
 μ 4 -O represents a tetradentate bridging oxido; 
 L j  represents at each occurrence independently from each other a ligand species; 
 a j  is at each occurrence independently from each other an integer from 1 to 100; 
 n is an integer from 2 to 10; 
 u is an integer from 2 to 100; 
 v is an integer from 0 to 100; 
 w is an integer from 0 to 100; 
 x is an integer from 0 to 100; 
 y is an integer from 0 to 100; and 
 z is an integer from 0 to 100. 
 
     
     
         18 . Formulation according to  claim 17 , wherein the following equation is fulfilled: 
       
         
           
             
               
                 
                   
                     4 
                     * 
                   
                   ⁢ 
                   u 
                 
                 - 
                 
                   [ 
                   
                     v 
                     + 
                     w 
                     + 
                     
                       
                         2 
                         * 
                       
                       ⁢ 
                       
                         ( 
                         
                           x 
                           + 
                           y 
                           + 
                           z 
                         
                         ) 
                       
                     
                     + 
                     
                       
                         ∑ 
                         
                           j 
                           = 
                           1 
                         
                         
                           j 
                           = 
                           n 
                         
                       
                         
                       
                         ( 
                         
                           
                             
                               
                                 m 
                                 j 
                               
                               ( 
                               
                                 L 
                                 j 
                               
                               ) 
                             
                             * 
                           
                           ⁢ 
                           
                             a 
                             j 
                           
                         
                         ) 
                       
                     
                   
                   ] 
                 
               
               = 
               c 
             
           
         
         wherein: 
         m j (L j ) represents the amount of negative charge of L j ; and 
         c represents the total charge of the titanium polyoxometalate (POM); 
         and a j , n, u, v, w, x, y, and z are defined as in  claim 17 . 
       
     
     
         19 . Formulation according to  claim 15 , wherein the one or more titanium polyoxometalates (POMs) are independently from each other selected from Ti 12  polyoxometalates, Ti 16  polyoxometalates, Ti 18  polyoxometalates, Ti 44  polyoxometalates, and Ti 52  polyoxometalates. 
     
     
         20 . Formulation according to  claim 15 , wherein the mass ratio of titanium polyoxometalates (POMs) in the formulation is in the range from 0.1% to 50% (w/w) based on the total mass of the formulation. 
     
     
         21 . Optical device comprising an optical metal oxide layer, which is obtainable by a method for preparing an optical metal oxide layer comprising the following steps:
 (a) providing a formulation comprising one or more titanium polyoxometalates (POMs) and one or more formulation media;   (b) applying the formulation to a surface of a substrate; and   (c) converting the formulation on the surface of the substrate to an optical metal oxide layer,
 or 
   
       which is prepared by using a formulation for preparing an optical metal oxide layer, wherein the formulation comprises:
 (i) one or more titanium polyoxometalates (POMs); 
 (ii) one or more formulation media; and 
 (iii) one or more additives selected from surfactants, wetting and dispersion agents, adhesion promoters, and polymer matrices, 
 wherein the optical device is preferably an augmented reality (AR) and/or virtual reality (VR) device.

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