IP Library Granted Patent US 10,290,385
Granted Patent B2
US 10,290,385 · App. 14/382,464 · Granted May 14, 2019

Synthetic diamond materials for electrochemical sensing applications

Inventors: Eleni Bitziou (West Midlands, GB); Laura Anne Hutton (Oxfordshire, GB); Julie Victoria MacPherson (West Midlands, GB); Mark Edward Newton (West Midlands, GB); Patrick Robert Unwin (West Midlands, GB); Nicola Louise Palmer (Oxfordshire, GB); Timothy Peter Mollart (Oxfordshire, GB); Joseph Michael Dodson (Berkshire, GB)
Assignee: Element Six Limited
H01B1/04G01N27/308
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Quick Facts
Patent No.
US 10,290,385
App. No.
14/382,464
Granted
May 14, 2019
Kind
B2
Abstract

A boron doped synthetic diamond material which has the following characteristics: a solvent window meeting one or both of the following criteria as measured by sweeping a potential of the boron doped synthetic diamond material with respect to a saturated calomel reference electrode in a solution containing only deionized water and 0.1M KNO 3 as a supporting electrolyte at pH 6: the solvent window extends over a potential range of at least 4.1 V wherein end points of the potential range for the solvent window are defined when anodic and cathodic current density measured at the boron doped synthetic diamond material reaches 38 mA cm −2 ; and the solvent window extends over a potential range of at least 3.3 V wherein end points of the potential range for the solvent window are defined when anodic and cathodic current density measured at the boron doped synthetic diamond material reaches 0.4 mA cm −2 ; a peak-to-peak separation ΔEp (for a macroelectrode) or a quartile potential ΔE 3/4 _ 1/4 (for a microelectrode) of no more than 70 mV as measured by sweeping a potential of the boron doped synthetic diamond material at a rate of 100 mV s −1 with respect to a saturated calomel reference electrode in a solution containing only deionized water, 0.1M KNO3 supporting electrolyte, and 1 mM of FcTMA + or Ru(NH 3 )6 3+ at pH 6; and a capacitance of no more than 10 μF cm −2 as measured by sweeping a potential of the boron doped synthetic diamond material with respect to a saturated calomel reference electrode between 70 mV and −70 mV in a solution containing only deionized water and 0.1M KNO 3 supporting electrolyte at pH 6, measuring resultant current, subtracting a current value at 0 V when sweeping towards negative potentials from a current value at 0 V when sweeping towards positive potentials, dividing the subtracted current value by 2, and then dividing the result by an area (cm 2 ) of the boron doped synthetic diamond material and by a rate at which the potential is swept (Vs −1 ) to give a value for capacitance in F cm −2 .

Claims (21)

1. A boron doped synthetic diamond material which has the following characteristics:

a solvent window meeting one or both of the following criteria as measured by sweeping a potential of the boron doped synthetic diamond material with respect to a saturated calomel reference electrode in a solution containing only deionised water and 0.1M KNO 3 as a supporting electrolyte at pH 6:

the solvent window extends over a potential range of at least 4.1 V wherein end points of the potential range for the solvent window are defined when anodic and cathodic current density measured at the boron doped synthetic diamond material reaches 38 mA cm −2 ; and

the solvent window extends over a potential range of at least 3.3 V wherein end points of the potential range for the solvent window are defined when anodic and cathodic current density measured at the boron doped synthetic diamond material reaches 0.4 mA cm −2 ;

a peak-to-peak separation ΔE p (for a macroelectrode) or a quartile potential ΔE 3/4-1/4 (for a microelectrode) of no more than 70 mV as measured by sweeping a potential of the boron doped synthetic diamond material at a rate of 100 mV s −1 with respect to a saturated calomel reference electrode in a solution containing only deionised water, 0.1M KNO 3 supporting electrolyte, and 1 mM of FcTMA + or Ru(NH 3 ) 6 3+ at pH 6; and

a capacitance of no more than 10 μF cm −2 as measured by sweeping a potential of the boron doped synthetic diamond material with respect to a saturated calomel reference electrode between 70 mV and −70 mV in a solution containing only deionised water and 0.1M KNO 3 supporting electrolyte at pH 6, measuring resultant current, subtracting a current value at 0 V when sweeping towards negative potentials from a current value at 0 V when sweeping towards positive potentials, dividing the subtracted current value by 2, and then dividing the result by an area (cm 2 ) of the boron doped synthetic diamond material and by a rate at which the potential is swept (V s −1 ) to give a value for capacitance in F cm −2 ,

wherein at least a portion of an exposed surface layer of the boron doped synthetic diamond material comprises boron doped synthetic diamond material having a boron content in a range 7×10 20 boron atoms cm −3 to 7×10 21 boron atoms cm −3 , and

wherein the boron doped diamond material does not exhibit non-diamond carbon peaks in a Raman spectrum of the boron doped diamond material.

2. A boron doped synthetic diamond material according to claim 1 , wherein the solvent window extends over at least a potential range of 4.3 V wherein end points of the potential range for the solvent window are defined when anodic and cathodic current density measured at the boron doped synthetic diamond material reaches 38 mA cm −2 .

3. A boron doped synthetic diamond material according to claim 2 , wherein the solvent window extends over at least a potential range of −2.1V to +2.2V.

4. A boron doped synthetic diamond material according to claim 1 , wherein the solvent window extends over at least a potential range of 3.4 V wherein end points of the potential range for the solvent window are defined when anodic and cathodic current density measured at the boron doped synthetic diamond material reaches 0.4 mA cm −2 .

5. A boron doped synthetic diamond material according to claim 1 , wherein ΔE p or ΔE 3/4-1/4 is no more than 66 mV.

6. A boron doped synthetic diamond material according to claim 1 , wherein the capacitance is no more than 8 μF cm −2 .

7. A boron doped synthetic diamond material according to claim 1 , wherein at least 50% of an exposed surface layer comprises boron doped synthetic diamond material having a boron content in a range 7×10 20 boron atoms cm −3 to 7×10 21 boron atoms cm −3 .

8. A boron doped synthetic diamond material according to claim 1 , wherein the exposed surface layer comprises boron doped synthetic diamond material having a boron content of no more than 3×10 21 boron atoms cm −3 .

9. A boron doped synthetic diamond material according to claim 1 , wherein the boron doped synthetic diamond material is a single crystal boron doped synthetic diamond material.

10. A boron doped synthetic diamond material according to claim 9 , wherein the single crystal boron doped synthetic diamond material comprises a capping layer having a boron content in a range 7×10 20 boron atoms cm −3 to 7×10 21 boron atoms cm −3 and a support layer having a lower boron content than the capping layer.

11. A boron doped synthetic diamond material according to claim 10 , wherein the support layer has a boron content of at least 5×10 18 boron atoms cm −3 .

12. A boron doped synthetic diamond material according to claim 9 , wherein a majority volume of at least 50% of the single crystal boron doped synthetic diamond material has a boron content in a range 7×10 20 boron atoms cm −3 to 7×10 21 boron atoms cm −3 .

13. A boron doped synthetic diamond material according to claim 9 , wherein an exposed surface of the single crystal boron doped synthetic diamond material comprises no more than 5% by area of crystallographic defects observable by visible microscopy at a magnification of up to ×100.

14. A boron doped synthetic diamond material according to claim 1 , wherein the boron doped synthetic diamond material is a polycrystalline boron doped synthetic diamond material.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 24, 2014
From: PALMER, NICOLA LOUISE; MOLLART, TIMOTHY PETER; DODSON, JOSEPH MICHAEL
To: ELEMENT SIX LIMITED
Reel/Frame 034250/0465 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 24, 2014
From: ELEMENT SIX LIMITED
To: ELEMENT SIX LIMITED
Reel/Frame 034250/0605 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 24, 2014
From: BITZIOU, ELENI; HUTTON, LAURA ANNE; MACPHERSON, JULIE VICTORIA; NEWTON, MARK EDWARD; UNWIN, PATRICK ROBERT
To: THE UNIVERSITY OF WARWICK
Reel/Frame 034251/0033 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 24, 2014
From: THE UNIVERSITY OF WARWICK
To: ELEMENT SIX LIMITED
Reel/Frame 034251/0205 →
Priority Claims (1)
GB 1204388.1 · Mar 13, 2012 · national
Continuity (2)
Provisional Application 61610286 · Mar 13, 2012
Related Publication 20150102266A1 · Apr 16, 2015