Conformal coating on three-dimensional substrates

Patent metadata

Field	Value
Publication number	US-10644302-B2
Application number	US-201515312176-A
Country	US
Kind code	B2
Filing date	May 20, 2015
Priority date	May 21, 2014
Publication date	May 5, 2020
Grant date	May 5, 2020

Abstract

The disclosure relates to a method for forming a conformal coating on a substrate having a topography presenting a relief. One method of the disclosure includes setting the temperature of the substrate within the range 140-275° C., and coating an aqueous solution including a sol-gel precursor on said substrate. The disclosure also relates to a method for fabricating a battery, a capacitor, a catalyst, a photovoltaic cell or a sensor using such a method, and to an aqueous solution for use in such a method.

First claim

The invention claimed is:

1. A method for forming a conformal coating on a substrate having a topography presenting a relief, said method comprising:
setting the temperature of the substrate within the range 140-275° C., and
coating an aqueous solution comprising a sol-gel precursor on said substrate to form a coated substrate; and
annealing the coated substrate to provide the conformal coating on the substrate having the topography presenting the relief,
wherein said relief is composed of a plurality of elements and at least one of said elements has an aspect ratio of at least 10,

wherein the conformal coating is a phase-pure TiO 2 anatase film, a lithium titanate film, a lithium lanthanum titanate film, a lithium tungstate film, or a lutetium iron oxide film.

2. The method according to claim 1 , wherein said aqueous solution further comprises a solvent which is water-miscible and suitable for lowering the surface tension of water, and wherein the solvent and the water are present in a volumetric ratio such as to set the surface tension of a mixture of water with said solvent in said ratio below 40 mM/m.

3. The method according to claim 1 , wherein at least one element of said relief has the shape of a pillar or a trench.

4. The method according to claim 1 , wherein the step of coating a solution is performed by spraying.

5. The method according to claim 4 , wherein said spraying is performed via an ultrasonic nozzle.

6. The method according to claim 1 , further comprising before the coating with the aqueous solution comprising the sol-gel precursor, cleaning said substrate with gaseous ozone in the presence of ultra-violet radiation.

7. A method for fabricating a battery, a capacitor, a catalyst, a photovoltaic cell or a sensor, comprising a step of forming a conformal layer on a substrate having a topography presenting a relief, according to the method as defined in claim 1 ; and assembling the conformal layer on the substrate into the battery, capacitor, catalyst, photovoltaic cell or sensor.

8. The method according to claim 1 , wherein the aqueous solution comprises:
water,
at least one metal oxide sol-gel precursor, said precursor being a metal carboxylate complex comprising at least a metal selected from the group consisting of Ti, Li, Fe, W, La and Lu, and at least an anion selected from the group consisting of citrate, glycolate, malate, lactate, tartrate, oxalate and acetate, and
a solvent which is water-miscible and suitable for lowering the surface tension of water,

wherein the solvent and the water are present in a volumetric ratio such as to set the surface tension of a mixture of water with said solvent in said ratio below 40 mN/m.

9. The method according to claim 8 , wherein said solvent is an alcohol.

10. The method according to claim 9 , wherein the alcohol is ethanol.

11. The method according to claim 9 , wherein the solvent to water ratio is from 0.7:1.0 to 1.5:1.0.

12. The method according to claim 8 , wherein said metal oxide sol-gel precursor comprises at least a metal selected from the group consisting of Li, Fe, W, La and Lu.

13. The method according to claim 12 , wherein said metal oxide sol gel precursor is a citrate metal precursor.

14. The method according to claim 1 , wherein the conformal coating is a phase-pure TiO 2 anatase film, a Li 4 Ti 5 O 12 spinel film, a Li 3x ,La( 2/3)-x ,TiO 3 film, a Li x ,WO 3 film, a phase-pure hexagonal LuFeO 3 film, or a phase-pure orthorhombic LuFeO 3 film.

15. The method according to claim 1 , wherein the annealing is performed at a temperature of from 450° C. to 1100° C.

16. The method according to claim 1 , wherein said aqueous solution further comprises a solvent which is water-miscible and suitable for lowering the surface tension of water, and wherein the solvent and the water are present in a volumetric ratio such as to set the surface tension of a mixture of water with said solvent in said ratio below 30 mN/m at 25° C.

17. The method according to claim 1 , wherein the sol-gel precursor is a metal carboxylate complex comprising at least a metal selected from the group consisting of Ti, Li, Fe, W, La and Lu, and at least an anion selected from the group consisting of citrate, glycolate, malate, lactate, tartrate, oxalate and acetate.

18. The method according to claim 1 , wherein the solvent is an alcohol and wherein the solvent and the water are present in a volumetric ratio of from 0.7:1.0 to 1.5:1.0.

19. The method according to claim 1 , wherein the conformal coating is a film of a lithium titanate, a lithium lanthanum titanate, a lithium tungstate, or a lutetium iron oxide.

20. The method according to claim 19 , wherein the conformal coating is a Li 4 Ti 5 O 12 spinel film, a Li 3x ,La( 2/3)-x ,TiO 3 film, a Li x ,WO 3 film, a phase-pure hexagonal LuFeO 3 film, or a phase-pure orthorhombic LuFeO 3 film.

21. The method according to claim 20 , wherein the step of coating a solution is performed by spraying and wherein said aqueous solution further comprises a solvent which is water-miscible and suitable for lowering the surface tension of water, and wherein the solvent and the water are present in a volumetric ratio such as to set the surface tension of a mixture of water with said solvent in said ratio below 30 mN/m at 25° C.

22. The method according to claim 1 , wherein the conformal coating has a thickness uniformity having a relative standard deviation of less than 5%.

Assignees

• Imec Vzw
• Univ Hasselt

Inventors

• Gielis Sven
• Hardy An
• Van Bael Marlies
• Vereecken Philippe M

Classifications

• H01M10/0585

  of accumulators having only flat construction elements, i.e. flat positive electrodes, flat negative electrodes and flat separators · CPC title

• C23C18/04

  Pretreatment of the material to be coated (C23C18/06 takes precedence) · CPC title

• H01M4/0419 Primary

  involving spraying · CPC title

• B05D1/02

  performed by spraying · CPC title

• C23C18/1245

  Inorganic substrates other than metallic · CPC title