CN115101357A - Preparation method and application of ternary nickel-cobalt-tungsten telluride composite material - Google Patents
Preparation method and application of ternary nickel-cobalt-tungsten telluride composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 25
- YCOASTWZYJGKEK-UHFFFAOYSA-N [Co].[Ni].[W] Chemical compound [Co].[Ni].[W] YCOASTWZYJGKEK-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 53
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000004744 fabric Substances 0.000 claims abstract description 52
- 229910017709 Ni Co Inorganic materials 0.000 claims abstract description 44
- 229910003267 Ni-Co Inorganic materials 0.000 claims abstract description 44
- 229910003262 Ni‐Co Inorganic materials 0.000 claims abstract description 44
- 239000002135 nanosheet Substances 0.000 claims abstract description 28
- 238000004070 electrodeposition Methods 0.000 claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 22
- 239000003792 electrolyte Substances 0.000 claims abstract description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 9
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 230000007547 defect Effects 0.000 claims abstract description 8
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 8
- 239000011206 ternary composite Substances 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007772 electrode material Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 8
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- 238000005406 washing Methods 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000000840 electrochemical analysis Methods 0.000 claims description 2
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- 238000001228 spectrum Methods 0.000 description 3
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- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002055 nanoplate Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
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- 229910052759 nickel Inorganic materials 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
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- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 1
- 150000004772 tellurides Chemical class 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- -1 transition metal tellurides Chemical class 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Abstract
The invention discloses a preparation method and application of a ternary nickel-cobalt-tungsten telluride composite material, which comprises the following steps: growing tungsten oxide nanosheets with oxygen defects on carbon cloth CC-WO 3‑x Chemically reacting with tellurium powder in hydrogen-argon mixed atmosphere at a certain temperature to obtain CC-WTE growing on carbon cloth 2 (ii) a The obtained CC-WTE 2 Obtaining CC-WTE in a three-electrode system through electrochemical deposition 2 -Ni-Co ternary composite, wherein, in a three-electrode system, the electrolyte is Ni (NO) 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 O mixed solution, working electrode CC-WTE 2 The reference electrode is an Ag/AgCl electrode, and the counter electrode is a Pt sheet electrode. The prepared CWNC-8 electrode has excellent electrochemical performance and the current density is 1A g ‑1 Specific capacitance 739F g ‑1 The capacity retention rate after 5000 cycles is 84%, which is 12% higher than that of CC-Ni-Co electrode. While the power density is 3000W kg ‑1 Then 23.4W h kg of the solution is remained ‑1 The energy density of (1).
Description
Technical Field
The invention relates to the technical field of electrode composite materials, in particular to a preparation method of a ternary nickel-cobalt-tungsten telluride composite material and application of the ternary nickel-cobalt-tungsten telluride composite material in an electrode material.
Background
Transition Metal Oxides (TMOs) composed of multiple metal elements generally have more excellent electrochemical performance, and can store more charges because various ions have more redox valence states. However, the single/multiple TMOs all face the defects that the self electronic conductivity is low, the structure is seriously collapsed after multiple charging and discharging, the service life is influenced, and the practical application is limited. At present, the research on material systems such as multi-element TMOs and sulfides is mature, the research on tellurides is relatively rare, and particularly the research on transition metal tellurides of multi-element systems is relatively rare. Due to the metal characteristics of tellurium and smaller electronegativity, the formed transition metal telluride has a narrower band gap structure and more excellent chemical stability, and is expected to be used as an excellent super capacitor SC electrode material. In the existing research, the performance of the TMO material is found to have a further improvement space, and the performance of the material can be further improved by preparing the composite material.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing a ternary nickel cobalt tungsten telluride composite material comprising the steps of:
step one, growing tungsten oxide nano-sheets CC-WO with oxygen defects on carbon cloth 3-x Chemically reacting with tellurium powder in hydrogen-argon mixed atmosphere at a certain temperature to obtain CC-WTE growing on carbon cloth 2 ；
Step two, the obtained CC-WTE 2 Obtaining CC-WTE in a three-electrode system through electrochemical deposition 2 -Ni-Co ternary composite, wherein, in a three-electrode system, the electrolyte is Ni (NO) 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 O mixed solution, working electrode CC-WTE 2 The reference electrode is an Ag/AgCl electrode, and the counter electrode is a Pt sheet electrode.
Preferably, in the first step, tungsten oxide nanosheets CC-WO having oxygen defects on carbon cloth are grown 3-x WO to 3-x The mass ratio of the tellurium powder to the tellurium powder is 3: 40-60; the tellurium powder and CC-WO 3-x The distance of (a) is 1-3 cm.
Preferably, in the first step, the chemical reaction is carried out in a high-temperature tube furnace, and the reaction temperature is as follows: heating to 600-700 ℃ at the speed of 1-3 ℃/min, and preserving the heat for 1-3 hours, wherein the volume fraction of Ar in the hydrogen-argon mixed atmosphere is 90%, and H 2 Is 10% by volume.
Preferably, in the second step, Ni (NO) is added 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 Dissolving O in distilled water to form electrolyte, and loading CC-WTE 2 Cutting the carbon cloth into 1cm multiplied by 1cm to be used as a working electrode, respectively using an Ag/AgCl electrode and a Pt sheet electrode as a reference electrode and a counter electrode, circulating for 5-15 circles within-1.2-0.2V at a scanning speed of 3-8 mV/s, and using deionized water and ethyl alcohol to obtain a sampleWashing with alcohol for 3-5 times, and drying in a vacuum drying oven at 50-70 ℃ for 10-15 h to obtain CC-WTE 2 -a Ni-Co ternary composite.
Preferably, the Ni (NO) 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 The mass ratio of O is 1: 1; the Ni (NO) 3 ) 2 ·6H 2 The mass-to-volume ratio of O to distilled water was 8mg:5 mL.
The invention also provides the ternary nickel-cobalt-tungsten telluride composite material prepared by the preparation method.
The invention also provides application of the ternary nickel-cobalt-tungsten telluride composite material prepared by the preparation method in an electrode material.
The invention also provides an electrochemical test method of the ternary nickel-cobalt-tungsten telluride composite material prepared by the preparation method, in a three-electrode system, the ternary nickel-cobalt-tungsten telluride composite material is used as a working electrode, Hg/HgO is used as a reference electrode, a Pt sheet is used as a counter electrode, 2M KOH is used as electrolyte, and a CHI660E electrochemical workstation is used for carrying out electrochemical performance test on the ternary nickel-cobalt-tungsten telluride composite material.
The tungsten oxide nanosheet CC-WO grown on carbon cloth and having oxygen defects 3-x The preparation method comprises the following steps: firstly, preparing a piece of 2cm × 5cm carbon cloth, sequentially cleaning the carbon cloth for 15 minutes by using deionized water and ethanol under ultrasonic waves, and then drying the carbon cloth; treating the dried carbon cloth with oxygen plasma for 15 minutes to increase the hydrophilicity of the surface of the carbon cloth; weigh 0.3g WCl 6 Dissolving in 60mL of glacial acetic acid, and stirring for 3h at room temperature to obtain a light yellow solution; putting the treated carbon cloth into the yellowish solution, transferring the obtained mixture into a 100mL stainless steel reaction kettle, sealing, carrying out solvothermal reaction in an oven at 180 ℃ for 12h, naturally cooling to room temperature, taking out the carbon cloth, fully washing the carbon cloth for 3-5 times by using absolute ethyl alcohol and deionized water, then putting the carbon cloth into the oven, drying at 60 ℃ for 12h to obtain WO with a layer of blue uniformly covered on the CC 3-x Sample (D) of (1), denoted as CC-WO 3-x 。
The invention at least comprises the following beneficial effects:
(1) successfully prepares the CC-WTE with a ternary composite structure on the carbon cloth by a high-temperature tellurization reaction and an electrodeposition method 2 -Ni-Co nanoplates, further improving the conductivity of the material; using CC-WTE 2 As a substrate, its synergistic interaction with Ni-Co nanoplates, CC-WTE 2 the-Ni-Co electrode realizes higher specific capacitance and cycle stability than the Ni-Co nanosheet directly grown on the carbon cloth alone, which is derived from the fact that the ternary mixed structure further improves the CC-WTE 2 The electronic conductivity of the Ni-Co electrode accelerates the redox reaction kinetics, and the cross-linked nanosheet structure exposes more electrochemical active sites, thereby providing a channel for the transmission of electrons and ions and greatly accelerating the transmission speed of the ions in the electrode material.
(2) The prepared CWNC-8 electrode has excellent electrochemical performance and the current density is 1A g -1 Specific capacitance 739F g -1 The retention rate of the capacitance after 5000 cycles is 84%, which is 12% higher than that of the CC-Ni-Co electrode. While the power density is 3000W kg -1 Then 23.4W h kg of the solution is remained -1 The energy density of (2).
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 shows CC-WTE with different magnifications 2 FESEM image of (a);
FIG. 2 is CC-WO of the present invention under different magnifications 3-x FESEM image of (a);
FIG. 3 shows FESEM images at different magnifications, wherein a-1 to a-3: CWNC-6; b-1 to b-3: CWNC-8; c-1 to c-3: CWNC-10;
FIG. 4 is a TEM image of the CWNC-8 of the present invention;
FIG. 5 is an XRD spectrum of a material prepared according to the present invention;
fig. 6 is a spectrum of CWNC-8 prepared in the present invention, wherein a: CWNC-8XPS full spectrum; b: te 3 d; c: w4 f; d: co 2 p; e: ni 2 p;
FIG. 7 shows CC-WTE prepared according to the present invention 2 CWNC-6, CWNC-8, CWNC-10 and CC-Ni-Co electrodes: a, b) at 30mV s -1 CV curve of lower, c, d) at 2A g -1 (iv) the lower GCD curve;
FIG. 8 is a) CV curve of CWNC-8 at different scan rates, b) GCD curve of CWNC-8 at different current densities, c) specific capacitance of CWNC-6, CWNC-8, CWNC-10 and CC-Ni-Co electrodes at different current densities, d) CC-WTE 2 EIS curves of CWNC-6, CWNC-8, CWNC-10 and CC-Ni-Co electrodes;
FIG. 9 shows a CWNC-8 electrode prepared according to the present invention: a) ragone graph, b) cycle life, c) cycle life of CC-Ni-Co electrode.
The specific implementation mode is as follows:
the present invention is described in further detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Tungsten oxide nanosheets CC-WO grown on carbon cloth with oxygen defects in the following examples 3-x The preparation method comprises the following steps: firstly, preparing a piece of 2cm × 5cm carbon cloth, sequentially cleaning the carbon cloth for 15 minutes by using deionized water and ethanol under ultrasonic waves, and then drying the carbon cloth; treating the dried carbon cloth with oxygen plasma for 15 minutes to increase the hydrophilicity of the surface of the carbon cloth; weigh 0.3g WCl 6 Dissolving in 60mL of glacial acetic acid, and stirring for 3h at room temperature to obtain a light yellow solution; putting the treated carbon cloth into the yellowish solution, transferring the obtained mixture into a 100mL stainless steel reaction kettle, sealing, carrying out solvothermal reaction in an oven at 180 ℃ for 12h, naturally cooling to room temperature, taking out the carbon cloth, fully washing the carbon cloth for 3-5 times by using absolute ethyl alcohol and deionized water, then putting the carbon cloth into the oven, drying at 60 ℃ for 12h to obtain WO with a layer of blue uniformly covered on the CC 3-x Sample (D) of (1), denoted as CC-WO 3-x 。
Example 1:
a preparation method of a ternary nickel-cobalt-tungsten telluride composite material comprises the following steps:
step one, preparing CC-WTE through a tellurization reaction in a high-temperature tube furnace 2 (ii) a Firstly, CC-WO 3-x (WO on carbon cloth 3-x About 30mg) and 500mg Te powder in the same quartz boat, the Te powder and CC-WO 3-x Approximately 2cm apart; before the start of the reaction, the tube furnace was subjected to three vacuum purges, after which argon and hydrogen were used as a shielding gas and a carrier gas (Ar 90%, H) 2 10%), set temperature program: raising the temperature to 650 ℃ at the temperature of 2 ℃/min (20min), and preserving the heat for 2h at the temperature; after the tellurization reaction is finished, the tube furnace is naturally cooled to room temperature to obtain the CC-WTE growing on the carbon cloth 2 (ii) a The mass of the carbon cloth before and after the tellurization reaction is weighed to obtain CC-WTE 2 Has a mass of 1.495mg/cm 2 ；
Step two, preparing electrolyte: separately weigh Ni (NO) 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 Dissolving 800mg of O in 500mL of distilled water respectively;
and (3) an electrodeposition process: will load CC-WTE 2 Cutting the carbon cloth into 1cm multiplied by 1cm to be used as a working electrode, using an Ag/AgCl electrode and a Pt sheet electrode as a reference electrode and a counter electrode, circulating for 6 circles within-1.2-0.2V at a scanning speed of 5mV/s, washing for 3-5 times by using deionized water and ethanol, and marking a sample obtained after drying as CC-WTE 2 -Ni-Co-6 (CMNC-6); the loading capacity of the active substance is 2.055mg/cm 2 ；
Example 2:
a preparation method of a ternary nickel-cobalt-tungsten telluride composite material comprises the following steps:
step one, preparing CC-WTE through a tellurization reaction in a high-temperature tube furnace 2 (ii) a Firstly, CC-WO 3-x (WO on carbon cloth) 3-x About 30mg) and 500mg Te powder in the same quartz boat, the Te powder and CC-WO 3-x Spaced approximately 2cm apart; before the start of the reaction, the tube furnace was subjected to three vacuum purges, after which argon and hydrogen were used as a shielding gas and a carrier gas (Ar 90%, H) 2 10%), temperature programming: raising the temperature to 650 ℃ at the temperature of 2 ℃/min (20min), and preserving the heat for 2h at the temperature; after the completion of the tellurization reaction, the tubeNaturally cooling the furnace to room temperature to obtain the CC-WTE growing on the carbon cloth 2 (ii) a The mass of the carbon cloth before and after the tellurization reaction is weighed to obtain CC-WTE 2 Has a mass of 1.495mg/cm 2 ；
Step two, preparing electrolyte: separately weigh Ni (NO) 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 Dissolving 800mg of O in 500mL of distilled water respectively;
and (3) an electrodeposition process: will load CC-WTE 2 Cutting the carbon cloth into 1cm multiplied by 1cm to be used as a working electrode, using an Ag/AgCl electrode and a Pt sheet electrode as a reference electrode and a counter electrode, circulating for 8 circles at a scanning speed of 5mV/s within-1.2-0.2V, washing for 3-5 times by using deionized water and ethanol, and marking a sample obtained after drying as CC-WTE 2 -Ni-Co-8 (CMNC-8); the loading capacity of the active substance is 2.245mg/cm 2 ；
Example 3:
a preparation method of a ternary nickel-cobalt-tungsten telluride composite material comprises the following steps:
step one, preparing CC-WTE through a tellurization reaction in a high-temperature tube furnace 2 (ii) a Firstly, CC-WO 3-x (WO on carbon cloth 3-x About 30mg) and 500mg Te powder in the same quartz boat, the Te powder and CC-WO 3-x Approximately 2cm apart; before the start of the reaction, the tube furnace was subjected to three vacuum purges, after which argon and hydrogen were used as a shielding gas and a carrier gas (Ar 90%, H) 2 10%), set temperature program: raising the temperature to 650 ℃ at the temperature of 2 ℃/min (20min), and preserving the heat for 2h at the temperature; after the tellurization reaction is finished, the tube furnace is naturally cooled to room temperature to obtain the CC-WTE growing on the carbon cloth 2 (ii) a The mass of the carbon cloth before and after the tellurization reaction is weighed to obtain CC-WTE 2 Has a mass of 1.495mg/cm 2 ；
Step two, preparing electrolyte: separately weigh Ni (NO) 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 Dissolving 800mg of O in 500mL of distilled water respectively;
and (3) an electrodeposition process: load CC-WTE 2 The carbon cloth is cut into 1cm multiplied by 1cm and then used as a working electrode, and an Ag/AgCl electrode and a Pt sheet electrode are used as parametersComparing the electrode and the counter electrode, circulating for 10 circles at a scanning rate of 5mV/s within-1.2-0.2V, washing for 3-5 times by using deionized water and ethanol, and obtaining a sample after drying, wherein the sample is marked as CC-WTE 2 -Ni-Co-8 (CMNC-8); the loading capacity of the active substance is 2.525mg/cm 2 ；
Comparative example 1:
step two, preparing electrolyte: separately weigh Ni (NO) 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 Dissolving 800mg of O in 500mL of distilled water respectively;
and (3) an electrodeposition process: cutting carbon cloth into 1cm multiplied by 1cm to be used as a working electrode, using an Ag/AgCl electrode and a Pt sheet electrode as a reference electrode and a counter electrode, circulating for 8 circles within-1.2-0.2V at a scanning speed of 5mV/s, washing for 3-5 times by deionized water and ethanol, and drying to obtain a sample which is marked as CC-Ni-Co-8;
CC-WTE obtained after high-temperature tellurization reaction 2 Is shown in fig. 1. CC-WTE 2 Retains the precursor CC-WO 3-x (FIG. 2) the same topographical features clearly show the presence of a large number of WTs on the carbon cloth 2 Sheet and WTE 2 WTE consisting of thin sheets 2 The hollow microsphere, the mixed nanostructure composed of the nano-sheet and the hollow microsphere is beneficial to the transmission of electrons and ions, and can improve the reaction kinetics. Then, use CC-WTE 2 The nano-sheets and the hollow microspheres are used as a supporting substrate and are further subjected to CC-WTE by an electrochemical deposition method 2 Growing Ni-Co nanosheets on the surface to obtain CC-WTE under different deposition times 2 SEM of-Ni-Co is shown in FIG. 3. FIG. 3 shows FESEM images of CWNC-6, CWNC-8 and CWNC-10 at different magnifications. As can be seen, CC-WTE was obtained after electrochemical deposition for various periods of time 2 -Ni-Co retains CC-WTE 2 And a partially hollow microsphere structure. At a short electrodeposition time, at CC-WTE 2 The surface of (A) is formed with non-uniform loose interconnected Ni-Co nano-sheets, as can be seen from FIGS. 3a-1 to a-3, the original CC-WTE 2 The hollow spherical structure of (2) is not completely opened (fig. 3 a), and as the electrodeposition time is increased to 8 circles, the interconnected porous Ni-Co nanosheets can be seen to uniformly cover the CC-WTe 2 And at this time, the original CC-WTE 2 Is fully open (fig. 3b-2), and CC-WTe can be seen in fig. 3b-1 and b-2 2 The lamella and the Ni-Co nanosheet structure are cross-linked with each other, no obvious hollow spherical structure exists, and the abundant void space is completely open at the moment. When the electrodeposition time is 10 circles, denser Ni-Co nanosheets can be observed from FIGS. 3c-1 to c-3, which may be associated with the increased electrodeposition time for the Ni-Co nanosheets in CC-WTE 2 In connection with the self-aggregation of the surface, this relatively dense structure may result in a slow rate of entry of electrolyte ions into the interior of the electrochemical material, possibly causing a reduction in electrochemical performance. FIGS. 3d-1 to d-3 are SEM images of CC-Ni-Co samples obtained by electrodeposition directly on carbon cloth. As the lamellar structure is obviously seen in the figure, the Ni-Co nanosheets grow unevenly on the surface of the carbon cloth and are obviously agglomerated locally, which may cause poor electrochemical performance. FIG. 4 is a transmission electron microscope image of CWNC-8 from which the lamellar porosity of the CWNC-8 electrode can be clearly seen.
The crystal structure of the obtained electrode material was characterized by XRD. FIG. 5 shows CC-WO 3-x ，CC-WTe 2 And an XRD pattern of CWNC-8. At CC-WTE 2 Can observe a wide peak of the carbon cloth at the 2 theta of 26 degrees, and belongs to WO 3-x The characteristic peak of (1) disappears, and the 2 theta of 12.5 degrees, 29 degrees, 29.8 degrees, 31.8 degrees, 34.2 degrees, 38.3 degrees, 41 degrees, 43.6 degrees, 47.3 degrees and 52.8 degrees respectively correspond to the (002), (104), (111), (013), (203), (006), (015), (301), (107) and (017) crystal faces of WTE2(JCPDS NO.81-1903), which indicates that CC-WTE is successfully obtained after high-temperature tellurization reaction 2 . And CC-WTE 2 All diffraction peaks in-Ni-Co are almost equal to those of CC-WTE 2 At the same position, no new additional diffraction peak appeared, and the strong diffraction peak around 34 ° at 2 θ became broad, indicating at CC-WTe 2 The Ni-Co nanosheet grown by electrodeposition has an amorphous structure. The amorphous structure is beneficial to improving the electronic conductivity, and further can improve the electrochemical performance.
The chemical composition and the valence state of the elements of the CWNC-8 sample were studied by XPS. XPS full of CWNC-8 samplesThe spectral images are shown in fig. 6a and contain six elements, C, Te, W, Co, Ni and O, the presence of which may result from oxidation or adsorption of oxygen on the surface of the sample exposed to air. FIG. 6b is an XPS spectrum of Te 3d, with peaks of Te 3d at around 575.9eV and 586.3eV 5/2 And 3d 3/2 Indicating that Te exists predominantly in the-2 valent form. FIG. 6c shows an XPS spectrum of W4f with two pairs of peaks in the W4f XPS spectrum, the two peaks at 35.3eV and 37.4eV corresponding to W 6+ 4f 5/2 And 4f 7/2 And the 33.0eV peak corresponds to W 4+ . The Co 2p peak of CWNC-8 fitted two satellite peaks, 795.8eV and 780.4eV, respectively, indicating that Co was +2 valent (FIG. 6 d). There are four peaks in the Ni 2p XPS spectra, as shown in FIG. 6e, where the two major peaks at 855.2 and 873.1eV belong to Ni 2p 1/2 And Ni 2p 3/2 Satellite peaks located adjacent to each major peak, unique to Ni 2p at 861.1 and 880.4eV, indicate that Ni is present at +2 valency in CWNC-8 samples.
The electrochemistry of all samples was evaluated using a standard three-electrode system with 2M KOH solution as the electrolyte. FIG. 7 shows CC-WTE 2 CWNC-6, CWNC-8 and CWNC-10 obtained after different electrodeposition cycles and CC-Ni-Co obtained by directly performing electrodeposition on carbon cloth at 30mV s -1 CV Curve of lower and at 2A g -1 GCD curve tested at current density. CC-WTE 2 The CV curve and the GCD curve of (C) visually indicate CC-WTE 2 Relatively inactive in the test system and contributes negligible to the overall specific capacitance of the electrode, CC-WTe 2 The porous channel is mainly used for constructing a porous channel, and good support is provided for the growth of nickel cobalt nanosheets at the later stage, so that the nickel cobalt nanosheets can be conveniently loaded. The CV and GCD curves of the CC-Ni-Co electrode obtained by directly growing the nickel-cobalt nanosheet on the carbon cloth show that when the scanning rate is increased to 30mV s -1 At this time, the shape of the curve is greatly changed due to the severe polarization effect (the inset in FIG. 7a shows CC-Ni-Co electrodeposited directly on carbon cloth at a scan speed of 10mV s -1 Lower CV curve), a similar phenomenon is observed in the GCD curve of CC-Ni-Co, the discharge curve and the charge curve of CC-Ni-Co are not completely symmetrical, anda large voltage drop was observed for CC-Ni-Co, indicating that the CC-Ni-Co electrode has poor electron conductivity and slow electron/ion transport kinetics, which may be associated with a porous structure that does not have open porosity and results in a large contact resistance after direct growth.
It can be seen from fig. 7 that CWNC-8 has the largest area of curve integration and the longest discharge time, indicating that CWNC-8 has the highest specific capacitance, which is mainly due to the synergistic effect of the rich hollow structure of the internal open channels of CWNC-8 and the Ni — Co nanosheets having high activity. Meanwhile, samples of CWNC-6, CWNC-8 and CWNC-10 were measured at 30mV s -1 All CV curves at the scan rate maintained a similar shape, but the redox peaks were slightly shifted due to polarization effects and slow transport of electrolyte/ions into the interior of the nanostructures. The results show that the constructed ternary tungsten nickel cobalt telluride nanosheet mixed nanostructure can obviously improve the electrochemical performance.
FIG. 8a shows a CWNC-8 electrode at 10-100 mV s -1 The CV curve under the scanning speed can be seen that a pair of redox peaks exist on the CV curve, which indicates that the Faraday redox reaction occurs in the energy storage process and has obvious pseudocapacitance characteristics. Notably, as the scan rate is increased to 70mV s -1 While the CV curve still maintains a pair of redox peaks without significant distortion, which means that the electrode has ideal electrochemical reversibility and excellent rate capability, as the scan speed continues to increase, the oxidation and reduction peaks move to higher positive and lower negative potentials, respectively, again due to polarization effects and slow transport of electrolyte/ions into the interior of the electrode material. CWNC-8 electrodes at different current densities (1-10A g) -1 ) The GCD results of the test are shown in figure 8 b. A clear plateau can be seen from the GCD curve, which means that the CWNC-8 electrode material has pseudo-capacitive behavior, belonging to the battery type electrode material, consistent with the CV curve results. Under different current densities, the discharge curve and the corresponding charge curve of the CWNC-8 electrode are almost symmetrical, which shows that the CWNC-8 has good oxidation-reduction reaction reversibility. According to GCD curves under different current densities, CWNC-6, CWNC-8, CWNC-10 and CWNC-10 are calculatedThe specific capacitance of the CC-Ni-Co electrode is shown in FIG. 8 c. It can be seen that CWNC-8 has the highest specific capacitance, and that the CWNC-8 electrode has current densities of 1, 2, 3, 5 and 10A g -1 When the specific capacitance is 740, 662, 613, 558, 484F g -1 And the specific capacitances of the CWNC-6, CWNC-10 and CC-Ni-Co electrodes are 431, 358, 336, 302 and 259F g in sequence under the same current density -1 610, 548, 376, 393, 345F g-1 and 403, 372, 343, 300, 265F g -1 Showing that the CC-WTE with the multi-component composition is performed under the proper electro-deposition time 2 The construction of the-Ni-Co nanosheet electrode material has higher conductivity and faster ionic and electronic transmission speeds, which can also be verified in EIS testing.
EIS was also used to study the electrochemical behavior of the electrode material, and the Nyquist curves for the five electrodes are shown in fig. 8d, with the inset showing a magnified view in the high frequency region. In general, the intersection point on the real axis of the high frequency region represents the internal resistance (Rs) of the electrode, and the Rs values of the five electrodes are shown in Table 1. It can be seen that in the high frequency region, the Rs of CWNC-8 and CWNC-10 is 0.398 Ω, which is the smallest of all samples, indicating the best conductivity, which indicates CC-WTE when the electrode material is constructed 2 The mixed nanostructure substrate and a certain amount of Ni-Co nano-sheets of (A) are indispensable, the Rs value of CWNC-8 and CC-WO 3-x (Rs 1.35 Ω), by a factor of 3.4. The high conductivity facilitates electron transfer and accelerates reaction kinetics, while CC-WTE2, CWNC-8 and CC-Ni-Co all have larger Rs values, indicating that they have larger contact resistance.
TABLE 1
| Sample (I) | CC-WTe2 | CWNC-6 | CWNC-8 | CWNC-10 | CC-Ni-Co |
| Rs | 1.641 | 2.110 | 0.398 | 0.398 | 1.321 |
The analysis shows that the electrodeposition time has great influence on the structure and the appearance of the electrode material, and further has great influence on the electrochemical performance. The optimal electrodeposition time was confirmed, and a CWNC-8 electrode having the best electrochemical performance was obtained. The excellent electrochemical performance of the CWNC-8 electrode is derived from proper Ni-Co nanosheets and CC-WTE 2 The mixed nanostructure and the construction of the multi-component are beneficial to ion diffusion and electron transfer, and the CWNC-8 electrode has higher conductivity and exposes more electrochemical active sites under the optimal electrodeposition time.
Based on the specific capacitance calculated from the three-electrode GCD test, the Energy Density (ED) and Power Density (PD) of CWNC-8 were further calculated. FIG. 9a shows a Ragon diagram of a CWNC-8 electrode at a current density of 1A g -1 And 10A g -1 The maximum energy density and power density obtained were 35.75 Wkg -1 (300W kg -1 ) And 3000W kg -1 (23.4W h kg -1 ). And under the same conditions, CC-WO 3-x The maximum power density of the electrode is 2602W kg -1 The energy density is 19.4W h kg -1 Indicates to react with CC-WO 3-x Compared with the electrode, the CWNC-8 electrode still retains higher energy density under higher power density.
FIGS. 9b and 9c show respectivelyCWNC-8 and CC-Ni-Co electrodes were measured at 50mV s -1 The long cycle stability of the CV test shows that the CWNC-8 has good cycle performance, after 5000 cycles, the capacitance retention rate of the CWNC-8 electrode is 84%, and the capacitance retention rate of the CC-Ni-Co electrode is only 72%, which indicates that the CWNC-8 has more excellent cycle stability.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (8)
1. The preparation method of the ternary nickel-cobalt-tungsten telluride composite material is characterized by comprising the following steps of:
step one, growing tungsten oxide nano-sheets with oxygen defects on carbon cloth, wherein the tungsten oxide nano-sheets are CC-WO 3-x Chemically reacting with tellurium powder in hydrogen-argon mixed atmosphere at a certain temperature to obtain CC-WTE growing on carbon cloth 2 ；
Step two, the obtained CC-WTE 2 Obtaining CC-WTE in a three-electrode system through electrochemical deposition 2 -Ni-Co ternary composite, wherein, in a three-electrode system, the electrolyte is Ni (NO) 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 O mixed solution, working electrode CC-WTE 2 The reference electrode is an Ag/AgCl electrode, and the counter electrode is a Pt sheet electrode.
2. The method for preparing the ternary nickel-cobalt-tungsten telluride composite material as set forth in claim 1, wherein in the first step, tungsten oxide nanosheets CC-WO having oxygen defects grown on carbon cloth 3-x WO to 3-x The mass ratio of the tellurium powder to the tellurium powder is 3: 40-60; the tellurium powder and CC-WO 3-x The distance of (2) is 1-3 cm.
3. The method of preparing a ternary nickel cobalt tungsten telluride composite as set forth in claim 1 wherein in said first step, the chemical reaction is carried out in a high temperature tube furnace at a reaction temperature of: heating to 600-700 ℃ at the speed of 1-3 ℃/min, and preserving the heat for 1-3 hours, wherein the volume fraction of Ar in the hydrogen-argon mixed atmosphere is 90%, and H 2 Is 10% by volume.
4. The method of claim 1, wherein in step two, Ni (NO) is added 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 Dissolving O in distilled water to form electrolyte, and loading CC-WTE 2 Cutting the carbon cloth into 1cm multiplied by 1cm to be used as a working electrode, respectively using an Ag/AgCl electrode and a Pt sheet electrode as a reference electrode and a counter electrode, circulating for 5-15 circles within-1.2-0.2V at a scanning speed of 3-8 mV/s, washing an obtained sample with deionized water and ethanol for 3-5 times, and then drying in a vacuum drying oven at 50-70 ℃ for 10-15 hours to obtain CC-WTE 2 -a Ni-Co ternary composite material.
5. The method of making a ternary nickel cobalt tungsten telluride composite as set forth in claim 4 wherein said Ni (NO) is 3 ) 2 ·6H 2 O and Co (NO) 3 ) 2 ·6H 2 The mass ratio of O is 1: 1; the Ni (NO) 3 ) 2 ·6H 2 The mass-to-volume ratio of O to distilled water was 8mg:5 mL.
6. A ternary nickel cobalt tungsten telluride composite material prepared by the preparation method according to any one of claims 1 to 5.
7. The application of the ternary nickel-cobalt-tungsten telluride composite material prepared by the preparation method of any one of claims 1 to 5 in an electrode material.
8. An electrochemical test method for the ternary nickel-cobalt-tungsten telluride composite material prepared by the preparation method according to any one of claims 1 to 5, characterized in that in a three-electrode system, the ternary nickel-cobalt-tungsten telluride composite material is used as a working electrode, Hg/HgO is used as a reference electrode, a Pt sheet is used as a counter electrode, 2M KOH is used as an electrolyte, and a CHI660E electrochemical workstation is used for carrying out an electrochemical performance test on the ternary nickel-cobalt-tungsten telluride composite material.
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