IP Library Granted Patent US 10,662,550
Granted Patent B2
US 10,662,550 · App. 15/801,759 · Granted May 26, 2020

Diamond nanostructures with large surface area and method of producing the same

Inventors: Hongjun Zeng (Naperville, IL); Nicolaie A. Moldovan (Plainfield, IL)
Assignee: JOHN CRANE INC.
C30B29/04C01B32/26C01P2002/30C01P2006/12
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Quick Facts
Patent No.
US 10,662,550
App. No.
15/801,759
Granted
May 26, 2020
Kind
B2
Abstract

A method for forming diamond nanostructures with large specific area can include forming porous diamond nanostructures by means of selectively etching sp 2 -bonded carbon and partially removing sp 3 -bonded carbon in nanocrystalline diamond (NCD) and ultrananocrystalline diamond (UNCD® diamond). The diamond nanostructures achieved from the disclosed method can include a long shaft surrounded by a school of barbs. The nanostructure can provide a significantly larger surface area than diamond without such a nanostructure and its fabrication provides relative ease of manufacture compared to traditional techniques.

Claims (29)

1. A method of fabricating a diamond nanostructure, comprising:

providing a substrate;

depositing a layer of polycrystalline diamond including sp 2 and sp 3 carbon on to the substrate; and

selectively removing sp 2 carbon and partially removing sp 3 carbon from the layer of polycrystalline diamond, thereby increasing surface area of the layer of polycrystalline diamond and forming a layer of featherlike diamond nanostructures, wherein the surface of the layer of polycrystalline diamond is made porous.

2. The method as recited in claim 1 , wherein the layer of polycrystalline diamond is a conductive layer of at least one of boron doped nanocrystalline diamond (BD-NCD) or boron doped ultrananocrystalline diamond (BD-UNCD diamond).

3. The method as recited in claim 1 , wherein the layer of polycrystalline diamond is conductive and is doped with dopants other than boron, including at least one of nitrogen and/or phosphorus.

4. The method as recited in claim 1 , wherein the layer of polycrystalline diamond has an average grain size of 50 nm or smaller.

5. The method as recited in claim 1 , wherein the layer of polycrystalline diamond has an average grain size of 100 nm or smaller.

6. The method as recited in claim 1 , wherein the layer of polycrystalline diamond has an average grain size of 20 nm or smaller.

7. The method as recited in claim 1 , wherein the sp 2 carbon is selectively removed and the sp 3 carbon is partially removed by an organic acid.

8. The method as recited in claim 7 , wherein the organic acid contains acetic acid or oxalic acid.

9. The method as recited in claim 1 , wherein an inorganic electrolyte is used separately or combined with the organic acid for removing sp 2 and sp 3 carbon.

10. The method as recited in claim 9 , wherein the inorganic electrolyte includes NaCl or Sulfuric acid.

11. The method as recited in claim 1 , wherein selectively removing sp 2 carbon includes selectively removing carbon by application of a positive voltage on the layer of polycrystalline diamond, whereby at least a portion of the carbon is etched off.

12. The method as recited in claim 11 , wherein application of a positive voltage includes applying a current density of 50-2500 mA/cm 2 to a cell including electrolyte and the layer of polycrystalline diamond.

13. The method as recited in claim 1 , wherein partially removing sp 3 carbon includes removing at least one whole diamond grain in the layer of polycrystalline diamond.

14. The method as recited in claim 1 , wherein partially removing sp 3 carbon includes partially removing mass from at least one face of at least one diamond grain in the layer of polycrystalline diamond.

15. The method as recited in claim 1 , wherein the substrate includes at least one of Si, Mo, Nb, Ta, Ti, W, conductive ceramics, and/or conductive carbides.

16. The method as recited in claim 1 , further comprising adjusting sp 2 /sp 3 ratio of the layer of polycrystalline diamond for ease of etching.

17. The method as recited in claim 1 , further comprising adjusting facet orientation in the layer of polycrystalline diamond for ease of etching.

18. The method as recited in claim 1 , wherein the sp 2 carbon is selectively removed and the sp 3 carbon is partially removed with one or more selective and/or preferential etching process including thermal oxidation, hot gas corrosion, reactive ion etching, plasma etching, laser ablation, ion beam etching, and/or a combination of these methods, wherein a substantial portion of diamond material remains.

19. The method as recited in claim 1 , further comprising ceasing selective removal of sp 2 carbon and partial removal of sp 3 carbon once the layer of polycrystalline diamond is formed into the layer of feather-like diamond nanostructures and before any substantial number of the feather-like diamond nanostructures are removed.

20. The method as recited in claim 1 , further comprising, after selective removal of sp 2 carbon and partial removal of sp a carbon from the layer of polycrystalline diamond, forming at least one of a capacitor, a supercapacitor, or a sensor electrode using the layer of polycrystalline diamond.

21. A method of fabricating a diamond nanostructure, comprising:

providing a substrate;

depositing a layer of polycrystalline diamond including sp 2 and sp 3 carbon on to the substrate; and

selectively removing sp 2 carbon and partially removing sp 3 carbon from the layer of polycrystalline diamond, thereby increasing surface area of the layer of polycrystalline diamond, wherein the surface of the layer of polycrystalline diamond is made porous and ceasing selective removal of sp 2 carbon and partial removal of sp 3 carbon are performed at a point during selective removal of sp 2 carbon and partial removal of sp 3 carbon when the surface area of the layer of polycrystalline diamond has increased to at least two times that of the layer of polycrystalline diamond prior to selective removal of carbon.

22. The method of claim 21 wherein the surface area has increased by a factor of 10 or more.

23. The method of claim 21 wherein the polycrystalline diamond layer after selective removing comprises featherlike diamond nanostructures.

Assignments (3)
CORRECTIVE ASSIGNMENT TO CORRECT THE EXECUTION DATE TO 4/17/2019 AND TO ADD APPL. NO. 14/431,653 PREVIOUSLY RECORDED ON REEL 050202 FRAME 0452. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT OF ASSIGNORS INTEREST. Recorded Aug 30, 2019
From: ADVANCED DIAMOND TECHNOLOGIES, INC.
To: JOHN CRANE INC.
Reel/Frame 050886/0837 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 28, 2019
From: ADVANCED DIAMOND TECHNOLOGIES, INC.
To: JOHN CRANE INC.
Reel/Frame 050202/0452 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 3, 2017
From: ZENG, HONGJUN; MOLDOVAN, NICOLAIE A.
To: ADVANCED DIAMOND TECHNOLOGIES, INC.
Reel/Frame 044028/0835 →