IP Library Granted Patent US 12,012,559
Granted Patent B2
US 12,012,559 · App. 15/977,831 · Granted Jun 18, 2024

Janus membranes via atomic layer deposition

Inventors: Ruben Waldman (Chicago, IL); Hao-Cheng Yang (Westmont, IL); Seth B. Darling (Chicago, IL)
Assignee: UCHICAGO ARGONNE, LLC
C10G33/06C01B32/168C02F2101/325C02F2305/08
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Quick Facts
Patent No.
US 12,012,559
App. No.
15/977,831
Granted
Jun 18, 2024
Kind
B2
Abstract

A Janus membrane exhibiting sides with different properties and methods of fabricating such a Janus membrane. The membrane comprises a polymer material lacking polar functional groups. One side of the membrane is masked during atomic layer deposition (ALD). ALD is utilized to deposit a conformal coating on an exposed side of the membrane.

Claims (34)

1. A method of fabricating a Janus membrane comprising:

positioning a membrane in a housing in an Atomic Layer Deposition (ALD) reactor, the membrane having a first side and a second side and comprising a material, the membrane positioned within the housing with the entire second side disposed on and physically masked from precursor exposure by a portion of the housing and the first side exposed to a reaction chamber of the ALD reactor, wherein the membrane lacks polar functional groups; and

depositing an oxide coating on the first side of the membrane and within a network of pores within the membrane by performing at least 150 cycles of atomic layer deposition, wherein a cycle of the at least 150 cycles comprises the steps of:

exposing a first ALD precursor flux comprising a first ALD precursor at a first deposition temperature, a first vapor pressure, and for a first exposure time;

absorbing the first ALD precursor to the first side of the membrane and within a portion of the network of pores;

a purge step, after absorbing the first ALD precursor, comprising a pulse of inert gas for purge time of between 10 seconds and 60 seconds;

after the purge step, exposing a second ALD precursor flux comprising water at a second deposition temperature, a second vapor pressure, and for a second exposure time;

reacting the absorbed first ALD precursor with the second ALD precursor; and

forming a coating on the first side and the portion of the network of pores;

wherein flow of the first ALD precursor in the network of pores is governed by Knudsen diffusion; and

wherein the deposition of the oxide coating forms a uniform thickness on the first side and a thickness gradient of oxide coating within the network of pores and further wherein the second side is free of the oxide coating.

2. The method of claim 1 , wherein the membrane is polypropylene.

3. The method of claim 1 , wherein the first ALD precursor is an organometallic precursor.

4. The method of claim 1 , wherein the network of pores is tortuous.

5. The method of claim 1 , wherein the second ALD precursor is water.

6. The method of claim 1 , wherein the housing comprises a fixture and a masking plate, the fixture engageable with the masking plate and the membrane retained within the housing.

7. The method of claim 1 , wherein the first deposition temperature is between 60° C. and 110° C.

8. The method of claim 1 , wherein the first vapor pressure is up to 1 Torr.

9. A method of fabricating a membrane comprising:

positioning a membrane lacking polar functional groups in a housing in an Atomic Layer deposition (ALD) reactor, the membrane having a first side and a second side, so that the second side of the membrane is disposed on and physically masked from precursor exposure by a portion of the housing; and

depositing an oxide on the first side of the membrane and within a network of pores within the membrane by atomic layer deposition by the steps of:

performing an ALD cycle of:

exposing a first ALD precursor flux comprising a first ALD precursor at a first deposition temperature, a first vapor pressure, and for a first exposure time;

absorbing the first ALD precursor to the first side of the membrane and within a portion of the network of pores;

exposing a second ALD precursor flux comprising a second ALD precursor at a second deposition temperature, a second vapor pressure, and for a second exposure time;

reacting the absorbed first ALD precursor with the second ALD precursor; and

forming a plurality of oxide seeds on the first side and the portion of the network of pores,

wherein the ALD cycle is repeated 100 to 300 times; and

wherein the oxide within the network of pores has a monotonically decreasing thickness gradient with increasing pore depth.

10. The method of claim 9 , wherein the membrane is polypropylene.

11. The method of claim 9 , wherein the coating is an oxide and wherein the first ALD precursor is an organometallic precursor.

12. The method of claim 9 , wherein the network of pores is tortuous.

13. The method of claim 9 , wherein the second ALD precursor is water.

14. The method of claim 9 , wherein exposing the second precursor flux occurs immediately after exposing the first precursor flux without an intervening purge step.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 18, 2020
From: WALDMAN, RUBEN
To: THE UNIVERSITY OF CHICAGO
Reel/Frame 054689/0298 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 25, 2020
From: DARLING, SETH B.; YANG, HAO-CHENG
To: UCHICAGO ARGONNE, LLC
Reel/Frame 052017/0861 →
CONFIRMATORY LICENSE Recorded Apr 16, 2019
From: UCHICAGO ARGONNE, LLC
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 048918/0821 →
Continuity (1)
Related Publication 20190345397A1 · Nov 14, 2019