IP Library Granted Patent US 9,126,227
Granted Patent B2
US 9,126,227 · App. 14/186,996 · Granted Sep 8, 2015

Thin layer chromatography plates and related methods of manufacture including priming prior to infiltration with stationary phase and/or precursor thereof

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Quick Facts
Patent No.
US 9,126,227
App. No.
14/186,996
Granted
Sep 8, 2015
Kind
B2
Abstract

In an embodiment, a method for manufacturing a thin layer chromatography (“TLC”) plate is disclosed. The method includes forming a layer of elongated nanostructures (e.g., carbon nanotubes), priming the elongated nanostructures with one or more adhesion priming layers, and at least partially coating the elongated nanostructures with a coating. The coating includes a stationary phase and/or precursor of a stationary phase for use in chromatography. The stationary phase may be functionalized with hydroxyl groups by exposure to a base or acid. The stationary phase may further be treated with a silane (e.g., an amino silane) to improve the performance of the TLC plate. Embodiments for TLC plates and related methods are also disclosed.

Claims (35)

1. A method for manufacturing a chromatography apparatus, the method comprising:

forming a catalyst layer on a substrate;

forming a layer of elongated nanostructures on the catalyst layer;

priming the elongated nanostructures to form a layer of primed elongated nanostructures by at least partially coating the elongated nanostructures with at least one adhesion priming layer for promoting subsequent deposition of a coating thereon; and

at least partially coating the primed elongated nanostructures with the coating, wherein the coating includes at least one member selected from the group consisting of aluminum, aluminum oxide, titanium, and titanium oxide.

2. The method as recited in claim 1 , further comprising exposing the coating to at least one of an acid or base in order to bond hydroxyl groups to the stationary phase.

3. The method as recited in claim 2 , further comprising exposing the stationary phase to a silane in order to bond silane groups to the stationary phase.

4. The method as recited in claim 3 , wherein the silane comprises an amino silane.

5. The method as recited in claim 4 , wherein the amino silane comprises 3-aminopropyltriethoxysilane.

6. The method as recited in claim 1 , further comprising, after the act of at least partially coating the primed elongated nanostructures with the coating, at least partially removing the elongated nanostructures.

7. The method as recited in claim 6 , wherein the act of priming the elongated nanostructures includes priming the elongated nanostructures with an adhesion priming layer comprising amorphous carbon having a thickness of not more than about 10 nm.

8. The method as recited in claim 7 , wherein the act of at least partially removing the elongated nanostructures also removes the adhesion priming layer comprising the amorphous carbon.

9. The method as recited in claim 6 , wherein the act of priming the elongated nanostructures comprises priming the elongated nanostructures with a first adhesion priming layer and a second adhesion priming layer, wherein the first and second adhesion priming layers include different materials.

10. The method as recited in claim 9 , wherein the first adhesion priming layer includes amorphous carbon and the second adhesion priming layer comprises alumina.

11. The method as recited in claim 10 , wherein the first adhesion priming layer comprising the amorphous carbon has a thickness of not more than about 10 nm.

12. The method as recited in claim 10 , wherein the act of at least partially removing the elongated nanostructures also removes the first adhesion priming layer comprising the amorphous carbon.

13. The method as recited in claim 1 , wherein forming a layer of elongated nanostructures on the catalyst layer comprises growing a layer of carbon nanotubes on the catalyst layer.

14. The method as recited in claim 1 , wherein the at least one material of the coating is selected from the group consisting of aluminum oxide and titanium oxide.

15. The method as recited in claim 14 , wherein at least partially coating the primed elongated nanostructures with the coating includes at least partially infiltrating the elongated nanostructures with the at least one material by atomic layer deposition or pseudo-atomic layer deposition.

16. The method as recited in claim 1 , wherein the catalyst layer, the elongated nanostructures, and the coating including at least one of a stationary phase or a precursor of a stationary phase form a zigzag pattern.

17. The method as recited in claim 1 , wherein the at least one adhesion priming layer comprises at least one material selected from the group consisting of silicon, silicon dioxide, silicon nitride, aluminum, aluminum oxide, titanium, titanium oxide, zirconium, and zirconium oxide.

18. The method as recited in claim 1 , wherein the act of priming the elongated nanostructures includes depositing the at least one adhesion priming layer via chemical vapor deposition or via a solution.

19. The method as recited in claim 1 , wherein the elongated nanostructures include carbon nanotubes.

20. A method for manufacturing a chromatography apparatus, the method comprising:

forming a layer of carbon nanotubes;

priming the carbon nanotubes to form a layer of primed carbon nanotubes by at least partially coating the carbon nanotubes with at least one adhesion priming layer for promoting subsequent deposition of a coating thereon; and

at least partially coating the primed carbon nanotubes with the coating, wherein the coating includes at least one member selected from the group consisting of aluminum oxide and titanium oxide.

21. The method as recited in claim 20 , wherein the at least one material of the coating is aluminum oxide.

22. The method as recited in claim 20 , wherein the at least one material of the coating is titanium oxide.

23. A method for manufacturing a chromatography apparatus, the method comprising:

forming a layer of carbon nanotubes;

at least partially coating the carbon nanotubes to form a layer of coated carbon nanotubes by at least partially coating the carbon nanotubes with at least one adhesion layer for promoting subsequent deposition of another coating thereon; and

at least partially coating the coated carbon nanotubes with the another coating, wherein the another coating includes at least one oxide material, selected from the group consisting of aluminum oxide and titanium oxide.

24. The method as recited in claim 23 , wherein the at least one oxide material includes titanium oxide.

25. The method as recited in claim 23 , wherein the at least one oxide material includes aluminum oxide.

Assignments (5)
SECURITY INTEREST Recorded Jul 18, 2025
From: US SYNTHETIC CORPORATION
To: KEYBANK NATIONAL ASSOCIATION
Reel/Frame 074973/0089 →
RELEASE OF SECURITY INTEREST IN PATENTS Recorded Jul 17, 2025
From: JPMORGAN CHASE BANK, N.A.
To: CHAMPIONX LLC; APERGY ESP SYSTEMS, LLC; APERGY BMCS ACQUISITION CORP; HARBISON-FISCHER, INC.; NORRIS RODS, INC.,; NORRIS RODS, INC.,; NORRISEAL-WELLMARK, INC.; PCS FERGUSON, INC.; QUARTZDYNE, INC.; US SYNTHETIC CORPORATION
Reel/Frame 072004/0019 →
RELEASE OF SECURITY INTEREST Recorded Jun 7, 2022
From: BANK OF AMERICA, N.A.
To: ACE DOWNHOLE, LLC; HARBISON-FISCHER, INC.; NORRIS RODS, INC.; PCS FERGUSON, INC.; QUARTZDYNE, INC.; SPIRIT GLOBAL ENERGY SOLUTIONS, INC.; THETA OILFIELD SERVICES, INC.; APERGY BMCS ACQUISITION CORP.; NORRISEAL-WELLMARK, INC.; US SYNTHETIC CORPORATION; WINDROCK, INC.
Reel/Frame 060305/0001 →
SECURITY INTEREST Recorded Jun 5, 2020
From: ACE DOWNHOLE, LLC; APERGY BMCS ACQUISITION CORP.; HARBISON-FISCHER, INC.; NORRIS RODS, INC.; NORRISEAL-WELLMARK, INC.; PCS FERGUSON, INC.; QUARTZDYNE, INC.; SPIRIT GLOBAL ENERGY SOLUTIONS, INC.; THETA OILFIELD SERVICES, INC.; US SYNTHETIC CORPORATION; WINDROCK, INC.
To: BANK OF AMERICA, N.A.
Reel/Frame 053790/0001 →
SECURITY AGREEMENT Recorded May 9, 2018
From: APERGY (DELAWARE) FORMATION, INC.; APERGY BMCS ACQUISITION CORP.; APERGY ENERGY AUTOMATION, LLC; HARBISON-FISCHER, INC.; NORRISEAL-WELLMARK, INC.; PCS FERGUSON, INC.; QUARTZDYNE, INC.; SPIRIT GLOBAL ENERGY SOLUTIONS, INC.; US SYNTHETIC CORPORATION; WINDROCK, INC.
To: JPMORGAN CHASE BANK, N.A.
Reel/Frame 046117/0015 →