Methods and systems for labeling and detecting defects in a graphene layer

Patent metadata

Field	Value
Publication number	US-9297768-B2
Application number	US-201314118006-A
Country	US
Kind code	B2
Filing date	Apr 18, 2013
Priority date	Apr 18, 2013
Publication date	Mar 29, 2016
Grant date	Mar 29, 2016

Abstract

Fluorophores or other indicators can be used to label and identify one or more defects in a graphene layer by localizing at the one or more defects and not at other areas of the graphene layer. A substrate having a surface at least partially covered by the graphene layer may be contacted with the fluorophore such that the fluorophore selectively binds with one or more areas of the surface of the underlying substrate exposed by the one or more defects. The one or more defects can be identified by exposing the substrate to radiation. A detected fluorescence response of the fluorophore to the radiation identifies the one or more defects.

First claim

What is claimed is:

1. A method to label one or more defects in a graphene layer, the method comprising:
providing a substrate having a surface at least partially covered by the graphene layer; and
contacting the substrate with an indicator that selectively binds with one or more areas of the surface of the substrate exposed by the one or more defects in the graphene layer to label the one or more defects.

2. The method of claim 1 , wherein contacting the substrate with the indicator comprises contacting the substrate with an indicator that includes one of a fluorophore, a dye, a radioisotope, or a quantum dot.

3. The method of claim 1 , wherein contacting the substrate with the indicator comprises contacting the substrate with an indicator that includes a fluorophore, the method further comprising:
exposing the substrate to radiation effective to generate a detectable fluorescence response from the fluorophore at the one or more areas of the surface exposed by the one or more defects; and
monitoring the fluorescence response of the fluorophore, wherein a detected fluorescence response identifies the one or more defects and an absence of the fluorescence response indicates an absence of the one or more defects.

4. The method of claim 3 , wherein exposing the substrate to radiation comprises:
irradiating the substrate with ultraviolet radiation having a wavelength of about 360 nm to about 440 nm.

5. The method of claim 3 , further comprising:
removing the fluorophore from the one or more areas of the surface exposed by the one or more defects.

6. The method of claim 1 , further comprising contacting the substrate with a rinse liquid one or more times after contacting the substrate with the indicator to remove any non-localized indicator from the graphene layer.

7. The method of claim 1 , wherein providing the substrate comprises providing a substrate that includes an inorganic polar substrate.

8. The method of claim 1 , wherein contacting the substrate with the indicator comprises contacting the substrate with an indicator that includes a fluorophore and the fluorophore includes a silane fluorophore having a Formula I:
C 16 H 9 —N═CH—(CH 2 ) X —CH═N—(CH 2 ) W —SiV (3-Z) [O(CH 2 ) Y CH 3 ] Z   (I)

wherein V is —H or —(CH 2 ) U CH 3 , U is an integer of from 0 to 2, W is an integer of from 0 to 3, X is an integer of from 0 to 3, Y is an integer of from 0 to 2, and Z is an integer of from 1 to 3.

9. The method of claim 8 , wherein the silane fluorophore includes C 16 H 9 —N═CH—(CH 2 ) 3 —CH═N—(CH 2 ) 3 —Si(OCH 2 CH 3 ) 3 .

10. The method of claim 1 , wherein contacting the substrate with the indicator comprises contacting the substrate with an indicator that includes a fluorophore and the fluorophore includes an aminopyrene derived fluorophore having a formula II:
C 16 H 9 —N═CH—(CH 2 ) X —CHO  (II);

and at least the one or more areas of the surface exposed by the one or more defects comprise an amino silane having a formula III:
NH 2 —(CH 2 ) W —SiV (3-Z) [O(CH 2 ) Y CH 3 ] Z   (III),

wherein V is —H or —(CH 2 ) U CH 3 , U is an integer of from 0 to 2, W is an integer of from 0 to 3, X is an integer of from 0 to 3, Y is an integer of from 0 to 2, and Z is an integer of from 1 to 3.

11. The method of claim 10 , further comprising contacting the substrate with the amino silane before contacting the substrate with the indicator that includes the fluorophore, the amino silane at least binding with the one or more areas of the surface exposed by the one or more defects.

12. The method of claim 10 , wherein the aminopyrene derived fluorophore includes C 16 H 9 —N═CH—(CH 2 ) 3 —CHO, and the amino silane includes aminopropyltriethoxysilane NH—(CH 2 ) 3 —Si[O(CH 2 )CH 3 ] 3 .

13. A system to label one or more defects in a graphene layer, the system comprising:
a substrate having a surface at least partially covered by the graphene layer; and
a first reservoir that contains a solution of an indicator that selectively binds with one or more areas of the surface of the substrate exposed by one or more defects to label the one or more defects in the graphene layer, and configured to contact the substrate with the solution of the indicator.

14. The system of claim 13 wherein the indicator includes a fluorophore, the system further comprising:
a radiation source configured to irradiate the substrate to generate a detectable fluorescence response from the fluorophore at the one or more areas of the surface exposed by the one or more defects; and
a detector to monitor the fluorescence response of the fluorophore, wherein a detected fluorescence response identifies the one or more defects and an absence of the fluorescence response indicates an absence of the one or more defects.

15. The system of claim 13 , wherein the indicator includes a fluorophore and the fluorophore includes a silane fluorophore having a Formula I:
C 16 H 9 —N═CH—(CH 2 ) X —CH═N—(CH 2 ) W —SiV (3-Z) [O(CH 2 ) Y CH 3 ] Z   (I)

wherein V is —H or —(CH 2 ) U CH 3 , U is an integer of from 0 to 2, W is an integer of from 0 to 3, X is an integer of from 0 to 3, Y is an integer of from 0 to 2, and Z is an integer of from 1 to 3.

16. The system of claim 15 , wherein the silane fluorophore includes C 16 H 9 —N═CH—(CH 2 ) 3 —CH═NSi(OCH 2 CH 3 ) 3 or C 16 H 9 —N═CH—(CH 2 ) 3 —CH═N—(CH 2 ) 3 —Si(OCH 2 CH 3 ) 3 .

17. The system of claim 14 , wherein the radiation source is configured to provide ultraviolet radiation having a wavelength of about 360 nm to about 440 nm.

18. The system of claim 14 , further comprising a heater configured to heat the substrate to a temperature sufficient to remove the fluorophore from the one or more areas of the surface of the substrate exposed by the one or more defects.

19. The system of claim 18 , wherein the heater is configured to heat the substrate to about 350° C. to about 400° C. in presence of one or more flowing gases.

20. The system of claim 13 , wherein the indicator includes a fluorophore and the fluorophore includes an aminopyrene derived fluorophore having a formula II:
C 16 H 9 —N═CH—(CH 2 ) X —CHO  (II);

and at least the one or more areas of the surface exposed by the one or more defects comprise an amino silane having a formula III:
NH 2 —(CH 2 ) W —SiV (3-Z) [O(CH 2 ) Y CH 3 ] Z   (III),

wherein V is —H or —(CH 2 ) U CH 3 , U is an integer of from 0 to 2, W is an integer of from 0 to 3, X is an integer of from 0 to 3, Y is an integer of from 0 to 2, and Z is an integer of from 1 to 3.

21. The system of claim 20 , further comprising a second reservoir that contains a solution of the amino silane that selectively binds with the one or more areas of the surface exposed by the one or more defects, and configured to contact the amino silane with the substrate before the substrate is contacted with the fluorophore.

22. The system of claim 20 , wherein the aminopyrene derived fluorophore includes C 16 H 9 —N═CH—(CH 2 ) 3 —CHO, and the amino silane includes aminopropyltriethoxysilane NH 2 —(CH 2 ) 3 —Si[O(CH 2 )CH 3 ] 3 .

23. A method to inspect a graphene layer for one or more defects, the method comprising:
providing an inorganic polar substrate having a surface at least partially covered by the graphene layer;
contacting the substrate with a fluorophore that selectively binds with one or more areas of the surface of the substrate exposed by the one or more defects in the graphene layer to label locations of the one or mor

Assignees

• Empire Technology Dev Llc

Inventors

• Yager Thomas A
• Miller Seth Adrian

Classifications

• G01N21/91 Primary

  using penetration of dyes, e.g. fluorescent ink · CPC title

• G01N21/77

  by observing the effect on a chemical indicator · CPC title

• G01N21/8422

  Investigating thin films, e.g. matrix isolation method · CPC title

• G01N21/64

  Fluorescence; Phosphorescence · CPC title

• G01N2021/8433

  Comparing coated/uncoated parts · CPC title