US20180312983A1 - Electrochemical exfoliation of 2d materials - Google Patents

Electrochemical exfoliation of 2d materials Download PDF

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US20180312983A1
US20180312983A1 US15/770,046 US201615770046A US2018312983A1 US 20180312983 A1 US20180312983 A1 US 20180312983A1 US 201615770046 A US201615770046 A US 201615770046A US 2018312983 A1 US2018312983 A1 US 2018312983A1
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carbon
electronically conducting
conducting material
bulk
materials
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Ian Kinloch
Robert Dryfe
Amr Abdelkader
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University of Manchester
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals

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  • the present invention relates to a method for the production of 2 D materials and related nanoplatelet structures.
  • 2D nanomaterials Since the discovery of the remarkable physical properties and chemical stability of graphene, two-dimensional (2D) nanomaterials have attracted significant interest, becoming one of the most active research areas of materials science.
  • the study of 2D materials was originally dominated by research into clays and later oxides but now extends beyond graphene to materials such as hexagonal boron nitride (h-BN), transition metal chalcogenides (TMCs) and carbides (MXene materials that are related to bulk MAX phases).
  • h-BN hexagonal boron nitride
  • TMCs transition metal chalcogenides
  • MXene materials that are related to bulk MAX phases.
  • a common feature of these 2D nanomaterials is that they have strong (in-plane) covalent bonds within each layer but interact with adjacent layers via weak bonds, leading the sheets to stack into 3-dimensional bulk crystals.
  • 2D nanomaterials are produced via bottom-up growth by methods such as chemical vapor deposition or by top-down approaches such as micromechanical cleavage or liquid exfoliation of the bulk layered crystals by ultra-sonication.
  • these routes are unable to produce large quantities and/or the products suffer from very small sheet size, making them unsuitable for many applications such as energy storage, composites, and catalysis.
  • the present inventors have found that, through the provision of a composite electrode comprising the bulk 2D material to be exfoliated and an electronically conducting material such as a metal, this problem can be overcome.
  • the presence of the metal in the composite body of the electrode enables efficient intercalation between the stacked 2D layers to provide efficient exfoliation and excellent mono and few layer non-carbon-based 2D materials. This has been demonstrated even with bulk 2D materials which are known to be good insulators such as h-boron nitride.
  • the inventors attribute the efficient exfoliation at least in part to the presence of the metal lowering the current needed to effect the intercalation, even in cases where the non-carbon-based 2D material is a semi-conductor.
  • Lower currents reduce electricity consumption, may reduce the occurrence of unwanted side effects and may be safer to scale commercially.
  • the resultant 2D crystals are significantly larger in size than any reported wet-chemical technology for mass production of 2D materials. Many of these materials are readily dispersible in various organic solvents such as NMP and DMF and offer a variety of potential uses.
  • the present invention relates to methods for the production of 2D materials and 2D material nanoplatelet structures from non-graphitic sources.
  • the 2D materials produced are not graphene or functionalized graphene.
  • the present invention provides a method for the production of non-carbon-based 2D materials and/or non-carbon-based 2D material nanoplatelet structures having a thickness of less than 100 nm in an electrochemical cell, wherein the cell comprises:
  • a negative electrode which comprises a non-carbon-based bulk 2D material and an electronically conducting material
  • the method comprises the step of passing a current through the cell.
  • the non-carbon-based bulk 2D material is electrochemically exfoliated to afford non-carbon-based 2D materials and/or non-carbon-based 2D material nanoplatelet structures having a thickness of less than 100 nm.
  • non-carbon-based bulk 2D material and electronically conducting material are suitably provided as an admixture or composite of flakes or powders.
  • the negative electrode is the electrode held at the most negative potential out of the two electrodes.
  • the negative electrode is commonly referred to in electrochemistry as the cathode.
  • a reference electrode may also be used.
  • the electrode comprising a non-carbon-based bulk 2D material and an electronically conducting material is provided as a composite comprising a binder.
  • Suitable binders include polymers.
  • PVA polyvinyl alcohol
  • cellulose cellulose
  • PANI polyaniline
  • PVDF polyvinylidene fluoride
  • suitable polymers may include those that are known to be soluble in water or other solvents, which may aid isolated of the final product.
  • the electrode may be provided as an admixture of a non-carbon-based bulk 2D material and an electronically conducting material (e.g. a metal) in a membrane or mesh, reducing or obviating the inclusion of a binder.
  • an electronically conducting material e.g. a metal
  • the electronically conducting material is a metal.
  • the metal is a transition metal.
  • the electronically conducting material is ferromagnetic. This assists removal of after exfoliation (a suspension of the exfoliated material may simply be stirred with a magnetic flea, to which the particles attach).
  • Suitable ferromagnetic materials include iron, nickel and cobalt. Suitable alloys may also be used. In some cases, the metal is nickel.
  • the method includes the step of preparing the electrode comprising a non-carbon-based bulk 2D material and an electronically conducting material such as a metal.
  • the method may comprising forming a pellet comprising a bulk 2D material powder, the electronically conducting material (e.g. metal) and a binder.
  • the method comprises:
  • the bulk 2D material and electronically conducting material are provided as powders.
  • the sintering step takes place at 150° C. or more, preferably at 200° C. or more; more preferably at 250° C. or more.
  • the pellet may be sintered under argon at about 300° C.
  • the invention provides a pellet comprising a non-carbon-based bulk 2D material powder, an electronically conducting material (e.g a metal) and a binder, for example, a pellet obtainable from steps i to v.
  • an electronically conducting material e.g a metal
  • a binder for example, a pellet obtainable from steps i to v.
  • the invention provides a method of preparing a pellet comprising a non-carbon-based bulk 2D material and an electronically conducting material (e.g a metal), the method comprising steps i to v detailed above.
  • the present invention provides a non-carbon-based 2D material or nanoplatelet structure obtainable by a method as described herein.
  • the term “2D material” is used to describe materials consisting of ideally one to ten layers, preferably where the distribution of the number of layers in the product is controlled.
  • the method can also be used to make 2D nanoplatelet structures under 100 nm in thickness, preferably under 10 nm in thickness and more preferably under 1 nm in thickness.
  • the size of the flakes produced can vary from nanometres across to millimetres, depending on the morphology desired.
  • the material produced is a 2D material having up to ten layers.
  • the 2D material produced may have one, two, three, four, five, six, seven, eight, nine or ten layers.
  • the material produced may comprise at least 10% by weight of 2D material having up to ten layers, preferably at least 25% by weight and more preferably at least 50% by weight of 2D material having up to ten layers.
  • the method produces primarily or only non-carbon-based 2D materials. In other cases, the method produces both non-carbon-based 2D materials and/or non-carbon-based 2D material nanoplatelet structures having a thickness of less than 100 nm. It will be appreciated that, under certain conditions, the method may produce primarily non-carbon-based 2D material nanoplatelet structures having a thickness of less than 100 nm. In other words, the average number of layers of the material produced may vary from mono and few layer to 10 or more layers.
  • Carbon-based 2D materials are becoming increasingly well-known. They feature sheets of fused six-membered carbocyclic rings in a honeycomb arrangement.
  • the most famous carbon-based 2D material is graphene, which is composed of planar sheets of unsaturated carbocyclic rings (benzenes) with a delocalised ⁇ electron system over the entire sheet.
  • Carbon-based 2D materials may also contain non-carbon groups, and the term carbon-based 2D materials includes these partially saturated and entirely saturated compounds.
  • graphane is a saturated carbon-based 2D material comprising sheets of fused 6-membered carbocycles in which each carbon bears a hydrogen atom. Both 1-sided and 2-sided graphane are known.
  • Other carbon-based 2D materials include, without limitation, graphene oxide and fluorographene.
  • Non-carbon based 2D materials do not include carbocyclic rings.
  • Examples of non-carbon-based 2D materials include hexagonal boron nitride (h-BN), transition metal chalcogenides (TMCs), and metal carbides.
  • the non-carbon-based 2D material of the present invention is 2D h-BN.
  • the non-carbon based 2D material of the present invention is a transition metal dichalcogenide (TMDC).
  • TMDCs include, without limitation, molybdenum disulfide (MoS 2 ), tungsten disulfide (WS 2 ), molybdenum diselenide (MoSe 2 ) and tungsten diselenide (WSe 2 ).
  • the non-carbon based 2D material of the present invention is a disulfide, for example, MoS 2 or WS 2 .
  • a bulk 2D material comprises many layers of 2D material stacked and held together with weak forces.
  • graphene is a 2D material
  • graphite is the corresponding bulk 2D material held together with Van der Walls forces.
  • bulk materials are used in the electrode that undergoes exfoliation. Exfoliation affords 2D materials and/or 2D material nanoplatelet structures. It will be appreciated bulk materials comprise many hundreds of layers, typically many thousands of layers.
  • cathode is used to refer to the negative electrode.
  • the cathode comprises a bulk non-carbon-based 2D material and an electronically conducting material.
  • the electronically conducting material is a ferromagnetic metal such as nickel.
  • the w/w ratio of bulk 2D material to electronically conducting material may be 5:1 to 1:1, for example 3:1 to 1:1, for example, 2.5:1 to 1.5:1. In some cases, the w/w ratio is about 2:1.
  • the electronically conducting material is provided as a powder.
  • the powder may be ⁇ m-sized or smaller, for example ⁇ 1 ⁇ m.
  • Suitable electrolytes are known in the art and include those described in WO2014/191765 (which is herein incorporated by reference in its entirety for all purposes, and in particular the section entitled electrolytes beginning on page 15).
  • Suitable electrolytes include salt solutions, molten salts, and ionic liquids such as eutectic systems.
  • Salt solutions may be solutions in aqueous solvents, in organic solvents or in eutectic solvents.
  • Eutectic systems are ionic liquids formed of a mixture of compounds having a melting point lower than that of the individual components. In some cases, the melting point of the eutectic system is at least 25° C. lower than that of lowest melting point component, for example at least 50° C. lower, at least 75° C. lower, preferably at least 100° C. lower.
  • Eutectic systems and solvents may include, for example, choline chloride (ChCl):Urea (1:2 M ratio), ChCl:Ethylene glycol (1:2), ChCl:Glycerol (1:2), ChCl:Malonic acid (1:1), ChCl:CrCl 3 .6H2O (1:3), ChCl:ZnCl 2 (1:2), ZnCl 2 :Urea (1:3.5), Ethylammonium chloride:Acetamide (1:1.5), EMC:Ethylene glycol (1:3), EMC:Glycerol (1:3), MPB:Ethylene glycol (1:3), MPB:Glycerol (1:3)
  • the electrolyte is a solution of an inorganic salt such as LiCl or an organic salt such as an alkylamine salt, for example trimethylamine hydrochloride or trimethylamine hydrochloride.
  • Suitable solvents may include DMSO.
  • the solvents are eutectic solvents.
  • the electrolyte may be a salt such as LiCl dissolved in a eutectic solvent such as a urea:choline chloride mixture (typically in a 2:1 mole ratio).
  • the electrolyte is a molten salt, for example NaCl or LiCl may be used so that the material can exfoliated at high temperatures of 600° C.+. It will be appreciated that the stability of the 2D material to be produced should be considered in selecting an upper temperature (as some are known to be unstable at high temperatures).
  • the electrode's binder may be pyrolised prior to use to increases its structural stability at this elevated temperatures.
  • the electrolyte is a eutectic system.
  • the electrolyte may be a eutectic mixture of a quaternary ammonium salt and a metal chloride. Suitable examples are provided above.
  • the positive electrode may consist of any suitable material known to those skilled in the art as it does not play a role in the material production, other than to provide a counter electrode for the anions.
  • the positive electrode is made from an inert material such as gold, platinum or carbon.
  • the positive electrode may be made of a material that oxidises to give the metal ions in the electrolyte, such as lithium.
  • the electrode surface area is as large as possible to prevent gas bubbles wetting it and/or disrupting the process at the negative electrode.
  • the positive and/or reference electrode may also be placed in a membrane or molecule sieve to prevent undesired reactions in the electrolyte or at either electrode.
  • the positive and the negative electrodes could alternatively be placed in a two-compartment cell, wherein each compartment contains one electrode, and the compartments are connected through a channel.
  • the working potential of the cell will be at least that of the standard potential for reductive intercalation.
  • An overpotential may be used in order to increase the reaction rate and to drive the cations into the galleries of the graphite at the negative electrode.
  • an overpotential of 1 mV to 10 V is used against a suitable reference as known by those skilled in the art, more preferably 1 mV to 5 V.
  • a larger potential may be applied across the electrodes but a significant amount of the potential drop will occur over the cell resistance, rather than act as an overpotential at the electrodes. In these cases the potential applied may be up to 20V or 30V.
  • both the electrodes comprise a non-carbon-based bulk 2D material and a metal and the potential is swept so that electrodes change from positive to negative and vice versa.
  • the cationic exfoliation would occur at both electrodes, depending on the polarity of the electrode during the voltage cycle.
  • alternating current can be used to allow for both fast intercalations and de-intercalations.
  • the current density at the negative electrode may be controlled using methods as are known in the art.
  • the cell is operated at a temperature which allows for production of the desired material.
  • the cell may be operated at a temperature of at least 10° C., preferably at least 20° C.
  • the maximum cell operating temperature may be 100° C., and more preferably 90° C., 80° C., 70° C. or 50° C. In some embodiments, the cell may be operated at a temperature of at least 30, 40, 50, 75, 100, 150 or even 200° C.
  • the maximum cell operating temperature may, in some cases, be as high as 250° C.
  • the optimum operating temperature will vary with the nature of the electrolyte. Operating the cell up to the boiling point of the electrolyte may be carried out in the present invention, keeping in mind the temperature stability of the desired product.
  • the cations used for the exfoliation are recovered after exfoliation.
  • the cations may be recovered by washing and/or heating of the exfoliated material, electrochemical reduction of the cations, ultrasonic energy treatment of the exfoliated material, displacement from the exfoliated material by surfactants or combinations thereof.
  • non-carbon-based 2D materials and non-carbon-based 2D material nanoplatelet structures having a thickness of less than 100 nm produced by the method of the invention may be separated from the electrolyte by a number of separation techniques, including:
  • the electrochemically exfoliated non-carbon-based 2D materials and non-carbon-based 2D material nanoplatelet structures may be further treated after exfoliation.
  • the materials may be further exfoliated using ultrasonic energy and other techniques known to those skilled in the art to decrease the flake size and number of layers.
  • the electrochemical intercalation may be repeated in order to achieve full exfoliation.
  • Raman spectroscopy can be used to measure the number of layers that a graphene flake possesses through the shape, intensity and position of the peaks.
  • non-carbon-based 2D materials may be analysed using Raman spectroscopy.
  • TEM and AFM images may also be used to determine flake size.
  • FIG. 1 shows a TEM image of the solution produced in example 1 spray-coated on silicon wafer and subjected to AFM analysis to confirm the exfoliation.
  • FIG. 2 shows the Raman spectra of the bulk (lower) and exfoliated (upper) MoS 2 of Example 1.
  • FIG. 3 shows an AFM image and measurements of a representative exfoliated flake of Example 2.
  • FIG. 4 shows the Raman spectra of exfoliated (lower) and bulk (upper) MoS 2 using a 633 nm excitation.
  • the exfoliated material was obtained in example 2.
  • FIG. 5 shows an AFM image and measurements of a representative exfoliated flake of Example 3.
  • FIG. 6 shows an AFM image and measurements of a representative exfoliated flake of Example 4.
  • FIG. 7 shows a TEM image of an exfoliated WS 2 nanosheet of Example 4 and the corresponding selected area electron diffraction (SAED) patterns.
  • Electrodes of WS 2 and other layered materials were prepared using similar protocols.
  • a cell was assembled with the MoS 2 pellets as cathode, and Pt wire as anode.
  • the liquid electrolyte was prepared by dissolving lithium chloride (Sigma Aldrich, 99.9%) and/or triethylamine hydrochloride in dimethyl sulfoxide (DMSO Sigma Aldrich, 99.9%). A potential of 10 V was applied for 10 hours.
  • the clear transparent electrolyte changes color to dark green due to suspension of the MoS 2 flakes in the electrolyte.
  • the suspension (about 30 ml) was then mixed with 2 L of water and stirred for 2 hours using a magnetic stirrer. During the stirring process, the Ni powder attached to the magnet, leaving the supernatant free of Ni. The solution was then centrifuged at 5000 rpm and the supernatant was decanted. The remaining powder was dried overnight under vacuum at 60° C.
  • the powder was then suspended in NMP by mild sonication for 20 minutes and diluted with ⁇ 30 isopropanol by volume.
  • the solution was then spray-coated on a silicon wafer and subjected to AFM analysis to confirm the exfoliation. Flakes with a thickness of ⁇ 1-3 nm were observed on the AFM images, indicating MoS 2 was exfoliated down to monolayer and few layers ( FIG. 1 ).
  • the size of the nanosheets ranged from 0.5 to 3 micron, which is 5-10 orders of magnitudes higher than the MoS 2 flakes produced by any previously reported liquid exfoliation method.
  • FIG. 2 shows the Raman spectra of the bulk and exfoliated MoS 2 . Both materials showed 2 bands at ⁇ 380 (A 1 g ) and ⁇ 405 (E 1 2 g ) cm ⁇ 1 . However, the difference between the 2 bands reduced from ⁇ 27 cm ⁇ 1 for the bulk to ⁇ 23 cm ⁇ 1 for the exfoliated materials. The intensity of the bands significantly enhanced after the exfoliation. Also full-widths at half-maximum values are obviously increased in the exfoliation products than in the bulk samples, which may be possibly attributed to phonon confinement by facet boundaries.
  • FIG. 3 shows an AFM image of a representative example of the exfoliated flake.
  • FIG. 4 shows the Raman spectra of exfoliated (lower) and bulk (higher) MoS 2 using the 633 nm excitation. It is clear that the bands of the exfoliated samples are different to that of the bulk material both in terms of Raman frequency and signal intensity.
  • the electrode was fabricated from h-BN powder.
  • the thickness of the obtained flake as measured by the AFM was below 5 nm for 80% of the flakes measured ( FIG. 5 ).
  • the electrode was fabricated from WS 2 powder.
  • the AFM confirmed the exfoliation of the bulk materials to few layers WS 2 ( FIG. 7 ).
  • the TEM image of exfoliated WS 2 nanosheets and the corresponding selected area electron diffraction (SAED) patterns are shown in FIG. 7 which indicate that the exfoliated TMDC materials still have a hexagonal lattice structure.
  • Raman spectra were obtained using a Renishaw system 1000 spectrometer coupled to a He—Ne laser (633 nm).
  • the laser spot size was ⁇ 1-2 ⁇ m, and the power was about 1 mW when the laser is focused on the sample using an Olympus BH-1 microscope.
  • the SEM images were taken using a Zeiss Leo 1530 FEGSEM.
  • TEM analysis was conducted using FEI Tecnai FZO 200 kv FEGTEM.
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EP3384068A1 (en) 2018-10-10
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