Inorganic porous coatings and methods of making the same

Patent metadata

Field	Value
Publication number	US-2023392254-A1
Application number	US-202217833841-A
Country	US
Kind code	A1
Filing date	Jun 6, 2022
Priority date	Jun 6, 2022
Publication date	Dec 7, 2023
Grant date	—

Abstract

Polymers of intrinsic microporosity are used herein as polymer templates for forming mechanical robust inorganic porous coatings that can be beneficially used as anti-reflective coatings.

First claim

1 . A process for forming an inorganic porous coating on a substrate, comprising:
forming a polymer template having a plurality of pores comprising applying a thin film of a polymer of intrinsic microporosity on the substrate; and performing an infiltration cycle comprising:
infiltrating the pores of the polymer template with a first vapor comprising a coating precursor material, wherein the coating precursor material is a precursor for forming an inorganic coating material and the coating precursor material binds to functional groups of the polymer template, and
infiltrating the pores of the polymer template having the coating precursor material bound thereto with a second vapor comprising a precursor reactant, wherein the bound coating material precursor reacts with the precursor reactant to form the inorganic coating material arranged to form the porous inorganic coating.

2 . The process of claim 1 , wherein forming the polymer template further comprises immersing the thin film in a solvent for a solvent treatment time.

3 . The process of claim 1 , further comprising removing the polymer of intrinsic microporosity after performing the infiltration cycle, thereby leaving the inorganic porous coating on the substrate

4 . The process of claim 1 , comprising performing from 1 to 20 infiltration cycles.

5 . The process of claim 1 , wherein the precursor reactant is H 2 O.

6 . The process of claim 1 , wherein the polymer of intrinsic microporosity is PIM-1.

7 . The process of claim 1 , wherein the thin film of the polymer of intrinsic microporosity has a thickness of about 20 nm to about 200 nm.

8 . The process of claim 1 , wherein the solvent is one or more of methanol, acetone, and toluene.

9 . The process of claim 1 , wherein the coating precursor material is one or more of trimethylaluminium (TMA), diethylzinc, tris(dimethylamido)silane, tetrakis(dimethylamido)zirconium, titanium tetrachloride, titanium tetraisopropoxide, nickel(II) acetylacetonate, palladium(II) hexafluoroacetylacetonate, copper bis(2,2,6,6-tetramethyl-3,5-heptanedionate, metallocenes having the formula (C 5 H 5 ) 2 M where M is Cr, Fe, Co, Ni, Pb, Zr, Ru, Rh, Sm, Ti, V, Mo, W, or Zn), and half-metallocene having the formula (C 5 H 5 )M(CH 3 ) 3 or (CH 3 C 5 H 4 )M(CH 3 ), wherein M is Cr, Fe, Co, Ni, Pb, Zr, Ru, Rh, Sm, Ti, V, Mo, W, or Zn).

10 . The process of claim 1 , wherein the inorganic coating has a porosity of about 10% to about 95%.

11 . (canceled)

12 . (canceled)

13 . (canceled)

14 . (canceled)

15 . (canceled)

16 . The process of claim 1 , wherein the substrate comprises a preexisting coating layer and the preexisting coating layer is one or more of an optical coating, a metal oxide layer, and a porous coating layer.

17 . (canceled)

18 . (canceled)

19 . A process for forming a multi-layer coating comprising: performing the process of claim 1 to form a first coating layer and repeating the process to form two or more additional coating layers on the first coating layer.

20 . (canceled)

21 . (canceled)

22 . A process for forming a multi-layer coating comprising:
forming a first porous inorganic coating layer on a substrate by the process of claim 1 ; and forming at least a second coating layer on the first porous inorganic coating layer.

23 . The process of claim 22 , wherein forming the second coating layer comprising:
forming a block copolymer polymer template having a plurality of pores on the substrate by applying a thin film of a block copolymer on the first porous inorganic coating layer and exposing the block copolymer thin film to a solvent treatment; and performing an infiltration cycle on the block copolymer template, comprising
infiltrating the pores of the block copolymer polymer template with a coating precursor material in a vapor phase, wherein the coating precursor material is a precursor for forming an inorganic coating material, and
infiltrating the pores of the block copolymer polymer template having the coating precursor material therein with a precursor reactant in a vapor phase, wherein the coating material precursor reacts with the precursor reactant to form the inorganic coating material arranged to form the second porous inorganic coating on the first porous inorganic coating, the second porous inorganic coating layer having tubular shaped pores.

24 . (canceled)

25 . (canceled)

26 . The process of claim 23 , further comprising removing the polymer of intrinsic microporosity before applying the thin film of the block copolymer.

27 . The process of claim 23 , further comprising removing the block copolymer after performing the infiltration cycle.

28 . (canceled)

29 . An anti-reflective coating formed by the process of claim 1 .

30 . A protective coating formed by the process of claim 1 .

31 . A porous inorganic multilayer coating formed on a substrate, comprising:
a first porous coating layer disposed on the substrate, the first porous coating layer comprising an inorganic oxide material and comprising a plurality of pores distributed substantially uniformly through the coating, the pores having an average pore size of less than about 10 nm as measured by electron microscopy; and a second porous coating layer formed from a block copolymer template arranged on the coating, wherein the second porous coating layer formed from the block copolymer comprises pores having a tubular pore structure.

32 . (canceled)

33 . (canceled)

34 . The multi-layer coating of claim 31 , wherein each of the coating layers has a different porosity.

35 .- 49 . (canceled)

Assignees

• Uchicago Argonne Llc
• Univ Chicago

Inventors

• Shevchenko Elena
• Guha Supratik
• Zhang Zhongbo
• Ji Cheng

Classifications

• C23C16/045 Primary

  Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates · CPC title

• C23C16/45553

  characterized by the use of precursors specially adapted for ALD · CPC title

• C23C16/403

  of aluminium, magnesium or beryllium · CPC title

• C09D5/006 Primary

  Anti-reflective coatings · CPC title

• C09D1/00

  Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances · CPC title