EP3044820A1 - Potential of zero charge modified carbon based electrode for desalination - Google Patents
Potential of zero charge modified carbon based electrode for desalinationInfo
- Publication number
- EP3044820A1 EP3044820A1 EP14843583.7A EP14843583A EP3044820A1 EP 3044820 A1 EP3044820 A1 EP 3044820A1 EP 14843583 A EP14843583 A EP 14843583A EP 3044820 A1 EP3044820 A1 EP 3044820A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- carbon
- solution
- electrode
- film
- formaldehyde
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Definitions
- This document relates generally to the field of conductive carbon-based electrodes and, more particularly, to an electrode comprising a carbon sheet coated with a film. This film leads to the relocation of carbon's potential of zero charge (PZC).
- PZC potential of zero charge
- Charge efficiency is one of the important performance terms for a capacitive deionization (CDI) cell, which is given by the ratio of the equivalent charge of salt adsorbed to the charge passed during the adsorption step.
- This efficiency value can be increased by variations in the applied voltage to the cell and the salt concentration, and the use of the membrane assisted electrodes. Beyond these physical variations/modifications, charge efficiency also can be alternatively elevated by chemically modifying the PZC of carbon-based electrodes. If the carbon's PZC is located in the electrode's working domain, a charge inefficiency will occur due to co-ion repulsion.
- an electrode comprising a carbon sheet coated with a film.
- This coated film results in the modification, or relocation, of the carbon's PZC.
- the carbon sheet comprises a conductive carbon-based material.
- the conductive carbon-based material is infiltrated with a solution comprising resorcinol and formaldehyde.
- the carbon- based material is woven and may comprise, for example, carbon cloth, carbon felt, or carbon yarn.
- a film is formed by dip-coating the carbon electrode in a solution followed by subsequent drying steps. The coating may have a thickness of between 1 A and 100 nm.
- a method for making an electrode comprises the steps of: (a) infiltrating a carbon-based material with a solution containing resorcinol and formaldehyde; (b) polymerizing the solution infiltrated onto the carbon-based material to obtain a polymerized material; (c) subjecting the polymerized material to a solvent-exchange process; (d) carbonizing the polymerized material to obtain a carbonized material; and (e) coating the carbonized material with a film.
- the subjecting step may include serially soaking the infiltrated carbon-based materialin deionized water and acetone followed by air drying.
- the method may include completing the carbonizing step at about 800 - 1100°C for 30 - 360 min. In one embodiment the carbonizing step is completed at about 1,000°C for about 120 minutes. In any embodiment, the carbonizing step may further comprise using a ramp rate of about 1 to 5°C min "1 for heating from and cooling to room temperature. Further, the carbonizing step includes using a N 2 or Ar gas supply with flow greater than 300 mL min "1 during carbonizing in order to provide an inert atmosphere.
- the solution used to infiltrate the carbon-based material has a mole ratio of resorcinol to formaldehyde of about 1:2.
- the coating step may further comprise dipping the carbonized carbon-based woven material into a silica solution.
- That silica solution may include tetraethyl orthosilicate.
- the solution includes tetraethyl orthosilicate, ethanol and nitric acid with a volumetric ratio of from 1: 1: 1 to 1:50: 1.
- the solution includes tetraethyl orthosilicate, ethanol and nitric acid with a volumetric ratio of from 1: 10: 1 to 1:30: 1.
- the solution includes tetraethyl orthosilicate, ethanol and nitric acid with a volumetric ratio of 1:20: 1.
- the coating step may comprise (a) dipping the carbonized woven carbon cloth into the silica solution, (b) drying the carbonized woven carbon cloth following dipping and (c) repeating steps (a) and (b).
- the dipping may be done for three minutes followed by drying for thirty minutes.
- the method may further comprise cutting the electrode to a desired shape.
- methods described herein are applied to a carbon-based woven material.
- the carbon-based woven material comprises carbon cloth, carbon felt, or carbon yarn.
- the carbon-based woven material comprises carbon cloth.
- the film is prepared from a solution comprising one or more of carbon nanotubes, silicon, organic-functionalized silicon, silica, organic-functionalized silica, copper, chitosan, alumina, titania, vanadia, zirconia, magnesia, any metal or metal oxide from any group 3 (IIIB) to group 12 (IIB) element, or any nonmetal.
- the film is prepared from a solution comprising one or more nonmetals, which are selected from the group consisting of silicon, germanium, boron, antimony, or tellurium.
- FIG. 2 indicates the use of TEOS modification (one of the modification methods) results in a significant change in the surface conditions. For instance, Si bonds were established on the carbon surface.
- FIG. 3 gives the FTIR results to attest the change in the functional groups at the surface of a carbon material before and after the modifications.
- FIG. 4 gives an example of relocation of the PZC for the treated sample by the use of sulfuric acid solution (SAS) and sulfanilic acid solution (SNAS). As indicated in the magnified plot, the degree of PZC shifting is -0.3 V when the unmodified (pristine) carbon is compared.
- SAS sulfuric acid solution
- SNAS sulfanilic acid solution
- FIG. 5 shows that not only the use of sulfuric acid solution (SAS) but also the used of electro-oxidative method results in the PZC region for the treated carbon being positively shifted.
- SAS sulfuric acid solution
- FIG. 6 shows the PZC region of a carbon material can be detected by both cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Both methods consistently suggest that the unmodified carbon (Pr) has a PZC region of ⁇ - 0.15 V vs SCE, and the treated sample (electro-oxidative) has a PZC region of -0.5 V vs. SCE.
- CV cyclic voltammetry
- EIS electrochemical impedance spectroscopy
- FIG. 7 shows that the PZC shifting of a carbon material can be achieved by the use of HNO 3 acid.
- the EIS spectra show the PZC region has been shifted from—0.2 V to -0.2 V after HNC -treatment.
- FIG. 8 shows the possible location of the PZC region of a carbon electrode within the respective potential distribution. This representation suggests that the deionization performance can be substantially boosted when the PZC region is out of the corresponding electrode's working domain, and vice versa. For example, when a CDI cell employs the treated carbon as the cathode and the untreated carbon as the anode, the separation performance indicated in FIG. 9 can be significantly enhanced.
- FIG. 1 illustrating a carbon sheet 10 which comprises a conductive woven carbon cloth infiltrated with a solution containing resorcinol and formaldehyde.
- that solution includes a mole ratio of resorcinol to formaldehyde in the range of from 5: 1 to 1:5.
- that solution includes a mole ratio of resorcinol to formaldehyde in the range of from 3: 1 to 1;3.
- that solution includes a mole ratio of resorcinol to formaldehyde of about 1:2.
- the infiltrated woven carbon cloth is subjected to polymerization. This is followed by subjecting the infiltrated woven carbon to a solvent exchange process. That solvent exchange process includes serially soaking the infiltrated woven carbon cloth with deionized water and acetone. This is then followed by air drying.
- the carbonizing is subjected to carbonizing.
- the carbonizing is completed at a temperature of between about 800 and about 1100°C for between about 30 and about 360 minutes.
- the carbonizing is completed at a temperature of between about 900 and about 1100°C for between about 60 and about 240 minutes.
- the carbonizing is completed at a temperature of between about 950 and 1050°C for between about 90 and about 180 minutes.
- the carbonizing is completed at about 1,000°C for about 120 minutes.
- the method may include using a ramp rate of about 1 to 5°C per minute for heating from and cooling to room temperature.
- the carbonizing is completed in an inert atmosphere.
- the inert atmosphere is provided by using a nitrogen gas supply with flow greater than 300 ml min "1 during carbonizing.
- the resulting carbon sheet 10 has a surface chemistry including carbon-carbon double bonds, carbon oxygen bonds and hydroxyl groups.
- the carbon sheet 10 is subjected to coating with a film.
- the carbon sheet 10 is dipped into a silica solution comprising tetraethyl orthosilicate (TEOS).
- TEOS tetraethyl orthosilicate
- the silica solution further comprises TEOS, ethanol and nitric acid with a volumetric ratio of 1:20: 1.
- the pH of the solution is between about 2 and 8 pH.
- the method includes (a) dipping the carbon sheet into the silica solution, (b) drying the carbon sheet following dipping and (c) repeating steps (a) and (b) until the silica coating is provided at a desired thickness. In one embodiment that thickness is between 1 A - 10 nm. In another embodiment that thickness is between 10 nm - 100 nm.
- the coating step further comprises dipping said carbonized material into said solution for 1 to 30 minutes and drying said carbonized material for 5 to 500 minutes. In a further embodiment, the dipping may be for three minutes followed by drying for thirty minutes.
- the dried film coated carbon sheet forms an electrode 12 (see Figure 2) including a unique surface chemistry. As illustrated in Figure 2, that surface chemistry includes -Si and -COOH functional groups which increase the negative charge on the surface of the electrode. This promotes cation absorption and thereby increases the wettability of the electrode 12 to provide for enhanced performance. This is particularly true for an electrode 12 utilized in capacitive deionization applications such as for the desalinition (e.g. , purification of salt water into drinking water.).
- the electrode described herein may be used in supercapacitors and/or batteries.
- the carbon sheets were composed of commercially conductive carbon cloth
- a solvent-exchange process was performed for the polymerized samples, in which the samples were subjected to 2-hours of soaking in deionized water, 2-hours of soaking in acetone, and 2-hours of air-drying. Finally, the samples were carbonized at 1000°C for 2 hours using a ramp rate of 1 or 5°C min 1 for both heating and cooling from room temperature using a nitrogen gas supply with flow greater than 300 ml/min.
- the quartz tube used here was 48 inches long with an external diameter of 3 inches and an internal diameter of 2.75 inches.
- the carbon sheets were modified by the following steps in order to lead to a silica film being formed at the carbon surface: TEOS (Sigma-Aldrich), ethanol (Pharmco-Aaper), and HNO 3 (Acros) were vigorously mixed with a volumetric ratio of 1:20: 1 in a sealed glass bottle for 1 hour at room temperature.
- the carbon sheets were dipped into the mixture for 3 min, and dried in an oven at 100°C for 30 min.
- the carbon sheets were dipped repetitively into the TEOS mixture so as to vary the amount of silica deposited. All the received carbon sheets were kept in a vacuum desiccator before any characterization.
- FTIR spectroscopy examined the chemical species at the carbon surface (FIG. 3).
- Table 2 Effect of Na 2 C0 3 addition on carbon xerogel sheets' porosities and surface area. The porosities and surface areas were calculated using BJH method based upon desorption isotherms.
- the PZC of the surface of an electrode as described herein may be modified to enhance deionization capability.
- Treatments for xerogel materials are shown using sulfuric acid (FIG. 4), sulfanilic acid (FIG. 4), and electrochemical oxidation (FIG. 5).
- Treatments for an activated carbon fiber cloth include electrochemical oxidation (FIG. 6) and nitric acid oxidation (FIG. 7). All of these treatments can be used with various carbon materials to shift the PZC and modify the salt removal capability of a capacitive deionization device.
- PZC shifting and ideal locations are showin in FIG. 8 with salt removal experiments for both capacitive deionization and membrane capacitive deionization being shown in FIG. 9.
- HNC -treatment The procedure for the HNC -treatment is as follows. A graduated cylinder with a film cover was used to heat 300 cm of -70% HNO 3 (Sigma- Aldrich) in a temperature-controlled coolant bath. When the temperature of HNO 3 was stable (at 20, 35, 50 and 80°C, selected by considering the principle of design of experiment), a carbon electrode, in one embodiment carbon xerogel (CX), with a geometric area of -70 cm was placed into the cylinder for 1 h. After treatment, to remove any residual HNO 3 on the surface of the carbon, the treated carbon was washed with a great amount of deionized water until the pH value approached neutral.
- CX carbon xerogel
- the wet carbon was post- treated at 160°C overnight in a vacuum oven before testing.
- the treated carbon electrodes can be labeled as C-20, -35, -50 and -80, representing carbon sheet that was treated in HN0 3 at different temperatures, e.g., C-20 means that a carbon sheet was treated at 20°C.
- C-20 means that a carbon sheet was treated at 20°C.
- Organic sulfanilic acid was also used to treat the carbon electrode.
- the procedure is as follows. A mixture of water (H 2 0), hydrochloric acid (HC1), sulfanilic acid (C 6 H 7 NO 3 S), sodium nitrite (NaN0 2 ), and acetone ((CH 3 ) 2 CO) in respective ratios of 39: 1.3: 1:0.4: 1.4 by weight was prepared in a beaker kept in a water bath with temperature at ⁇ 6°C.
- a carbon electrode, in one embodiment a CX sheet was placed in the reaction product and left to sit for 12 hours. The CX sheet was withdrawn and repeatedly rinsed in deionized water until the solution pH was neutral.
- a carbon electrode is heated at 350°C for between 0.5 h and 4 h in an oven or furnace open to the air.
- the corresponding samples can be denoted as C-Ox-(0.5h) and C-Ox-(4h).
- This oxidation leads to the creation of oxide groups on the carbon electrode's surface which positively shifts the electrode's PZC.
- Temperatures above 300°C and below 800°C can be used for various time durations to modify the extent to which the PZC is shifted which will affect the resulting deionization performance of a capacitive deionization (CDI) cell.
- CDI capacitive deionization
- the electrodes can be oxidized using electrochemical treatments.
- carbon electrodes can be electrochemically oxidized at the anode using a cell potential of 1.5 V in a CDI cell for a period of 20 hours with a 4 mM NaCl electrolyte solution.
- this cell potential can be anywhere from 0.4 V to 3 V for various time durations.
- This anode or positive electrode in this cell will subsequently have a positively-modified PZC which can be used to enhance deionization capacity in an asymmetrically configured CDI cell.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
Claims
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201361876264P | 2013-09-11 | 2013-09-11 | |
US201361915794P | 2013-12-13 | 2013-12-13 | |
US14/230,668 US20150166372A1 (en) | 2013-12-13 | 2014-03-31 | Electrode made from xerogel sheet coated with silica film |
PCT/US2014/054947 WO2015038612A1 (en) | 2013-09-11 | 2014-09-10 | Potential of zero charge modified carbon based electrode for desalination |
Publications (2)
Publication Number | Publication Date |
---|---|
EP3044820A1 true EP3044820A1 (en) | 2016-07-20 |
EP3044820A4 EP3044820A4 (en) | 2017-08-23 |
Family
ID=56116146
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP14843583.7A Withdrawn EP3044820A4 (en) | 2013-09-11 | 2014-09-10 | Potential of zero charge modified carbon based electrode for desalination |
Country Status (2)
Country | Link |
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EP (1) | EP3044820A4 (en) |
CN (1) | CN105706277A (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111430672B (en) * | 2020-04-03 | 2021-06-04 | 陕西科技大学 | Preparation method and application of silicon dioxide/carbon cloth self-supporting electrode material |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8629076B2 (en) * | 2010-01-27 | 2014-01-14 | Lawrence Livermore National Security, Llc | High surface area silicon carbide-coated carbon aerogel |
US9576694B2 (en) * | 2010-09-17 | 2017-02-21 | Drexel University | Applications for alliform carbon |
US8865351B2 (en) * | 2011-03-14 | 2014-10-21 | Ut-Battelle, Llc | Carbon composition with hierarchical porosity, and methods of preparation |
US8790814B2 (en) * | 2012-02-16 | 2014-07-29 | Nanotek Instruments, Inc. | Inorganic nano sheet-enabled lithium-exchanging surface-mediated cells |
-
2014
- 2014-09-10 CN CN201480061435.5A patent/CN105706277A/en active Pending
- 2014-09-10 EP EP14843583.7A patent/EP3044820A4/en not_active Withdrawn
Non-Patent Citations (4)
Title |
---|
J. J. WOUTERS ET AL: "Low Surface Area Carbon Fiber Electrodes Coated with Nanoporous Thin-Films of -Al2O3 and SiO2: Relationship between Coating Conditions, Microstructure and Double Layer Capacitance", JOURNAL OF THE ELECTROCHEMICAL SOCIETY, vol. 159, no. 8, 20 July 2012 (2012-07-20), US, pages A1374 - A1382, XP055354779, ISSN: 0013-4651, DOI: 10.1149/2.056208jes * |
JING LIU ET AL: "Graphene/carbon cloth anode for high-performance mediatorless microbial fuel cells", BIORESOURCE TECHNOLOGY, ELSEVIER BV, GB, vol. 114, 24 February 2012 (2012-02-24), pages 275 - 280, XP028422578, ISSN: 0960-8524, [retrieved on 20120314], DOI: 10.1016/J.BIORTECH.2012.02.116 * |
RYOO M-W ET AL: "Improvement in capacitive deionization function of activated carbon cloth by titania modification", WATER RESEARCH, ELSEVIER, AMSTERDAM, NL, vol. 37, no. 7, 1 April 2003 (2003-04-01), pages 1527 - 1534, XP004411236, ISSN: 0043-1354, DOI: 10.1016/S0043-1354(02)00531-6 * |
See also references of WO2015038612A1 * |
Also Published As
Publication number | Publication date |
---|---|
EP3044820A4 (en) | 2017-08-23 |
CN105706277A (en) | 2016-06-22 |
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