Patent

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Patent

ELECTROCHEMICAL DEVICES COMPRISING GRAPHENE

Drawings

Patent drawings and their descriptions. Click a drawing to enlarge it.

FIG. 1

FIG. 1 is a schematic diagram of a cu rr ent theory of operation for the disclosed method of making graphene.

FIG. 2

FIG. 2 is a digital image of the results from the cu rr ent method utilizing paraﬃn and 3.5 grams (2), 2.0 grams (4), and 0.5 grams (6) of sulfur.

FIG. 3

FIG. 3 is a digital image of the results from the cu rr ent method utilizing motor oil and 5.0 grams (10), 2.0 grams (12), 1.0 grams (14), 0.10 grams (18) of …

FIG. 4

FIG. 4 is a digital image of the results from the cu rr ent method utilizing mineral oil and with 5.0 grams (20), 2.0 grams (22), 1.0 grams (24), 0.10 grams …

FIG. 5

FIG. 5 is a digital image of the results from the cu rr ent method utilizing cyclohexanol and 5.0 grams sulfur (30), as well as no sulfur (32).

FIG. 6

FIG. 6 is a diagram illustrating a closed system, which is utilized in particular embodiments of the disclosed method.

FIG. 7

FIG. 7 is a digital image of an outer crucible containing graphene produced from rooﬁng cement using an embodiment of the method disclosed herein.

FIG. 8

FIG. 8 is an optical image from a microscope illustrating an exfoliated sample of graphene made using a particular embodiment of the disclosed method.

FIG. 9

FIG. 9 is an optical image from a microscope of exfoliated graphene made using motor oil and 5.0 grams of sulfur.

FIG. 10

FIG. 10 is an optical image from a microscope of exfoliated ﬂakes of graphene made using mineral oil and 3.5 grams of sulfur.

FIG. 11

FIG. 11 is a spectrum obtained from Raman analysis of a graphene sample made using a particular embodiment of the disclosed method.

FIG. 12

FIG. 12 is a spectrum obtained from Fourier transform-infrared spectroscopic analysis (FT- I R) of graphene on a germanium disk.

FIG. 13

FIG. 13 is a spectrum obtained from x-ray photoelectron spectroscopic (XPS) analysis of a graphene sample made using a particular embodiment of the disclosed …

FIG. 14

FIG. 14 is a spectrum obtained from x-ray photoelectron spectroscopic (XPS) analysis of a graphene sample made using a particular embodiment of the disclosed …

FIG. 15

FIG. 15 is a XPS spectrum of the C i s core level state of graphene.

FIG. 16

FIG. 16 is a 2-dimensional image illustrating the atomic structure of graphene made by the current method.

FIG. 17

FIG. 17 is a micrograph (0.7 x 0.7 nm 3 D) of graphene obtained from a particular embodiment of the cu rr ent method.

FIG. 18

FIG. 18 is an image illustrating line analysis of topography showing the periodicity of atomic structure of graphene.

FIG. 19

FIG. 19 is an image produced by a scanning electron microscope (SEM) illustrating graphene ﬂakes made using a particular embodiment of the disclosed method. FI …

FIG. 20

FIG. 20 is a SEM image of the edge of a graphene sample produced by working embodiments, illustrating its layered characteristics (also illustrated in

FIG. 21

FIG. 21 is a digital image illustrating an approximately 25 mm diameter graphene ﬂake made using a particular embodiment of the disclosed method.

FIG. 22

FIG. 22 is an optical micrograph (400x) illustrating the disclosed graphene material in water.

FIG. 23

FIG. 23 is an optical micrograph (400x) illustrating graphene layers of an embodiment of the disclosed graphene material.

FIG. 24

FIG. 24 is a TEM image showing layered characteristics of an embodiment of the disclosed graphene material on a nanometer scale.

FIG. 25

FIG. 25 is a thermogram of percent weight loss (Y-axis) versus temperature in degrees Celsius (X- axis).

FIG. 26

FIG. 26 is an image produced by a scanning electron microscope (SEM) illustrating layers of graphene made using a particular embodiment of the disclosed method.

FIG. 27

FIG. 27 is an image produced by a scanning electron microscope (SEM) illustrating diatoms coated with graphene using an embodiment of the method disclosed …

FIG. 28

FIG. 28 is an image produced by a scanning electron microscope (SEM) illustrating uncoated diatoms.

FIG. 29

FIG. 29.

FIG. 30

FIG. 30 is an expanded view of the image of

FIG. 31

FIG. 31 is an optical image of large graphene sheets ﬂoating on the surface of water.

FIG. 32

FIG. 32 is an SEM image of a graphene ﬂake on a copper grid.

FIG. 33

FIG. 33 is a TEM image of graphene ﬁlm, illustrating layers.

FIG. 34

FIG. 34 is a 3-dimensional AFM image of graphene.

FIG. 35

FIG. 35 is a 2-dimensional AFM image of graphene for an 8 m x 8 m scanning area.

FIG. 36

FIG. 36 is an image illustrating the height proﬁle of a particular graphene sample.

FIG. 37

FIG. 37 is a micron scale AFM of an embodiment of the disclosed graphene material, with a co rr esponding height proﬁle.

FIG. 38

FIG. 38 is a Raman spectrum obtained from thermogravimetric analysis, illustrating the peak obtained at 600 *C.

FIG. 39

FIG. 39 is a Raman spectrum obtained from thermogravimetric analysis, illustrating the peak obtained at 400 C.

FIG. 40

FIG. 40 is a Raman spectrum obtained from thermogravimetric analysis, illustrating the peak obtained at 550 C.

FIG. 41

performance graph

FIG. 41 is a graph of the Ferrari amorphization trajectory as applied to an embodiment of the disclosed graphene material.

FIG. 42

FIG. 42 is a graph that correlates each stage of

FIG. 43

FIG. 43 is a schematic diagram that illustrates the diﬀerences between electron transfer rates for edge-based transfers and for basal plane transfers.

FIG. 44

performance graph

FIG. 44 is a graph of cu rr ent (A) versus potential (m V vs. Ag/AgCl) and illustrates cyclic voltammograms of Ru(NH₃) 63+/2+ and Fe(CN) 63-4- with a 1 cm2 …

FIG. 45

FIG. 45 is an image illustrating the defects associated with the disclosed graphene material in comparison to an HOPG sample.

FIG. 46

performance graph

FIG. 46 is a graph of cu rr ent (g A/cm 2) versus potential (V vs. Ag/AgCl) and illustrates cyclic voltammograms of an embodiment of the graphene anode …

FIG. 47

performance graph

FIG. 47 is a graph of cu rr ent (g A/cm 2) versus potential (V vs. Ag/AgCl) and illustrates cyclic voltammograms of an embodiment of the graphene anode …

FIG. 48

performance graph

FIG. 48 is a graph of cu rr ent (g A/cm 2) versus potential (V vs. Ag/AgCl) and illustrates a cyclic voltammogram obtained from a pyrolytic graphite electrode …

FIG. 49

performance graph

FIG. 49 is a graph of cu rr ent (g A/cm 2) versus potential (V vs. Ag/AgCl) and illustrates cyclic voltammograms of an embodiment of the graphene anode …

FIG. 50

performance graph

FIG. 50 is a combined graph illustrating cyclic voltammograms of pyroltic graphite and the disclosed graphene material.

FIG. 51

FIG. 51 is a schematic illustration of co rr osion initiation through intercalation observed in HOPG and further illustrates the features of the disclosed …

FIG. 52

FIG. 52 is a schematic diagram illustrating an embodiment of a method of making a graphene anode according to the present disclosure.

FIG. 53

FIG. 53 is a digital image of an embodiment of the graphene anode disclosed herein.

FIG. 54

performance graph

FIG. 54.

FIG. 55

FIG. 55 is pseudo-ﬁrst order decay graph obtained from the degradation curve illustrated in

FIG. 56

performance graph

FIG. 56 is a graph of current (mA/cm 2) vs. potential (V vs. Ag/AgCl) illustrating a cyclic voltammogram of an embodiment of the disclosed graphene anode in 1 …

FIG. 57

FIG. 57 is an image of an embodiment of the disclosed graphene material before a stress test used to assess the material's corrosion resistance.

FIG. 58

FIG. 58 is an image of the embodiment of

FIG. 59

FIG. 59 is an image of a graphene material sample obtained using an embodiment of the disclosed method before a pitting corrosion stress test.

FIG. 60

FIG. 60 is an image of the graphene material sample of

FIG. 61

FIG. 61 is a cyclic voltammogram obtained from an embodiment of the disclosed graphene anode after being subjected to a four day constant potential stress test.

FIG. 62

FIG. 62 is a cyclic voltammogram exhibiting the capacitance characteristics of an embodiment of the disclosed graphene electrode.

FIG. 63

FIG. 63 is a cyclic voltammogram exhibiting the capacitance characteristics of an embodiment of the disclosed graphene electrode that has been anodized.

Claims

Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.

6 independent · 21 dependent

2
Independent
/02/17 1 2/0 2 8 A l lorn ey Reference Number 7832-85293-04 Application Number 14/166,717 Listing of Claims
3
Dependent← claim 1electrochemical device
The electrochemical device of claim 1, wherein the electrochemical device is used to store energy or to provide energy.
4
Dependent← claim 1grapheneelectrochemical device
The electrochemical device of claim 1, wherein the graphene layer provides a capacitance ranging from at least 200 [F/cm 2 to about 700 F/cm 2.
5
Dependent← claim 1grapheneelectrochemical device
(Original) The electrochemical device of claim 1, wherein the graphene layer is coupled to the positively charged electrode or the negatively charged electrode by an adhesive or a component that facilitates adhesion.
1. 6
  Dependent← claim 5adhesive (synthetic polymer or epoxy)electrochemical device
  The electrochemical device of claim 5, wherein the adhesive is a synthetic polymer, an epoxy, or a combination thereof.
2. 9
  Dependent← claim 5electrochemical device
  The electrochemical device of claim 5, wherein the component that facilitates adhesion is an organic solvent.
11
Dependent← claim 1grapheneelectrochemical device
The electrochemical device of claim 1, wherein the grain size is about 5 nm.
12
Dependent← claim 1graphenepolymer electrode substrateelectrochemical device
The electrochemical device of claim 1, wherein the positively charged electrode or the negatively charged electrode comprises a polymer onto which the graphene layer is deposited or coupled.
1. 13
  Dependent← claim 12organic polymer (polypropylene, polyvinyl chloride, or polyethylene)electrochemical device
  The electrochemical device of claim 12, wherein the polymer is an organic polymer selected from polypropylene, polyvinyl chloride, polyethylene, or combinations thereof.
2. 14
  Dependent← claim 12polystyreneelectrochemical device
  The electrochemical device of claim 12, wherein the positively charged electrode or the negatively charged electrode polymer is polystyrene.
15
Dependent← claim 1grapheneaqueous ultracapacitor
The electrochemical device of claim 1, wherein the device is an aqueous ultracapacitor and wherein the graphene layer provides a capacitance ranging from at least 200 F/cm 2 to about 700 F/cm 2 and the aqueous ultracapacitor produces from about 500 J/cm 2 to about 600 J/cm 2 of stored energy.
1. 16
  Dependent← claim 15aqueous ultracapacitor
  The electrochemical device of claim 15, wherein the aqueous ultracapacitor is symmetric or asymmetric.
2. 17
  Dependent← claim 15grapheneaqueous ultracapacitor
  The electrochemical device of claim 15, wherein the graphene is anodized.
3. 18
  Dependent← claim 15grapheneaqueous ultracapacitor
  The electrochemical device of claim 15, wherein the capacitance of the graphene ranges from about 250 F/cm 2 to about 675 F/cm 2.
4. 19
  Dependent← claim 15graphenenanomaterial (e.g., nanosprings)aqueous ultracapacitor
  The electrochemical device of claim 15, wherein the graphene is coupled to a nanomaterial.
5. 20
  Dependent← claim 15aqueous ultracapacitor
  The electrochemical device of claim 15, wherein the aqueous ultracapacitor produces about 550 J/cm 2 of stored energy.
21
Dependent← claim 1graphenegraphene anode
(Cu rr ently Amended) The electrochemical device of claim 1, wherein: the electrochemical device is positively charged electrode is a graphene anode comprising a graphene layer comprising graphene having a substantially micro-crystalline grain size ranging from about 2 nm to about 15 nm, basal planes that are substantially planar, and exhibits an anodic potential of at least 2 volts to about 3 volts; and further comprising wherein the graphene anode further comprises a support layer.
22
Independentgrapheneelectrochemical devicegraphene anode
Claims 22 and 23. SVG 14166717.02-02-2017.IYOZ₇₆₁CRXEAPX1.CLM.2.svg 0.16 4.4 Black and white passing non-potable water between a graphene anode and a cathode, wherein the graphene anode comprises graphene having a substantially micro crystalline grain size ranging from about 2.0 nm to about 15 nm, basal planes that are substantially planar, and exhibits an anodic potential of at least 2 volts to about 3 volts through an electrochemical device comprising a positively charged electrode; a negatively charged electrode; a graphene layer covering at least a portion of the positive electrode, the negative electrode, or both, the graphene layer comprising graphene having a substantially micro-crystalline grain size ranging from about 2 nm to about Page 4 of 7 02/02/17 12/028 Attorney Reference Number 7832-85293-04 Application Number 14/166,717 nm, basal planes that are substantially planar, and a total electrochemical window of from at least about 3 V to about 5 V; and an electrolyte; applying an electric current using a power source; and isolating potable water. canceled
23
Independent
canceled
25
Dependent← claim 24water remediation cell
(Withdrawn-Currently Amended) The method of claim 24, wherein the graphene anode and the cathode positively charged electrode and the negatively charged electrode of the electrochemical device are provided in a cell comprising an inlet through which the non-potable water enters the cell, and an outlet through which the potable water exits the cell.
26
Dependent← claim 24graphenegraphene anode
(Withdrawn-Currently Amended) The method of claim 24, wherein the graphene anode positively charged electrode is a graphene anode graphene having a substantially micro-crystalline nm, basal planes that are substantially planar, and to about 3 volts, and wherein the graphene anode contaminants in the non-potable water.
27
Independent
Claims 27-29. Page 5 of 7 canceled
28
Independent
canceled
29
Independentgraphene
canceled comprising a graphene layer comprising grain size ranging from about 2 nm to about exhibits an anodic potential of at least 2 volts is capable of decomposing one or more organic

Device structures

Layer stacks claimed or described, ordered top of device to substrate.

electrochemical device

negatively_charged_electrodenegatively charged electrode

electrolyteelectrolyte

graphenegraphene layer

positively_charged_electrodepositively charged electrode

aqueous ultracapacitor

electrolyteaqueous electrolyte

Materials

Materials described outside the worked examples.

graphene

Electrode Active Material

electrolyte

Electrolyte

Process steps

Additional fabrication and treatment steps described in the patent.

Graphene Synthesis

Step 1

Process details

precursors:carbonaceous starting material, sulfur

description:Heating carbonaceous material and sulfur to a temperature and for a time effective to produce graphene

Materials:graphene

Characterization

Measurements and analyses referenced in the patent, with their drawing references.

raman spectroscopy

Raman Spectroscopy

FIG. 11 is a spectrum obtained from Raman analysis of a graphene sample made using a particular embodiment of the disclosed method.

Figure references

FIG. 11

graphenegraphene

Reported properties

Performance values and ranges asserted in the specification or claims.

Property	Value	Material
graphene layer capacitance (claimed range)	200–700 F/cm2	graphene
aqueous ultracapacitor stored energy (claimed range)	500–600 J/cm2

Why these are connected

Related documents with shared materials, methods, properties, or citations.

ELECTROCHEMICAL DEVICES COMPRISING GRAPHENE | Matter42 Literature