CN108203095B - Tungsten carbide nano array material, preparation method and application thereof - Google Patents
Tungsten carbide nano array material, preparation method and application thereof Download PDFInfo
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
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Abstract
The invention discloses a tungsten carbide nano array material, which comprises a substrate material and a tungsten carbide nano array structure material grown on the substrate material, wherein the tungsten carbide nano array structure material can be nitrogen-doped or non-nitrogen-doped; the tungsten carbide nano array structure comprises a nano line array, a nano belt array, a nano columnar array or a nano webbed array. The invention also discloses a preparation method of the tungsten carbide nano array material and application of electrocatalytic hydrogen evolution and oxygen evolution and efficient photo-thermal evaporation water purification.
Description
Technical Field
The invention belongs to the field of preparation and utilization of inorganic nano materials, and particularly relates to a tungsten carbide nano array material, and a preparation method and application thereof.
Background
Tungsten carbide (WC) is cheap, is often used for preparing hard metals, and has stable properties. In air, it is stable at temperatures below 400 ℃. Tungsten carbide has good electrical and thermal conductivity. Research shows that the tungsten carbide has a plasma resonance effect and is resistant to laser irradiation. Tungsten carbide is stable in an acid system and has catalytic hydrogenolysis similar to that of platinum, and the hydrogenolysis can be expanded to the fields of organic catalysis and electrocatalysis. Due to the characteristics, the research on the tungsten carbide material is receiving wide attention, and the tungsten carbide material is also increasingly applied to the fields of production, life and military industry.
However, the preparation of tungsten carbide nano-materials currently faces a number of problems. First, the tungsten carbide nano material is mostly powder material, however, the powder material needs to be re-dispersed, sintered, sprayed, etc. in practical application, and the sprayed tungsten carbide material cannot be in good contact with the substrate, which all cause adverse effects in application, such as specific surface area, hardness, conductivity, etc. after the material is formed. Secondly, the preparation of tungsten carbide requires a high temperature carbonization process, which mostly uses a mixture of hydrogen and methane as a carbon source, making the production process dangerous. Thirdly, reported synthesis methods which do not use hydrogen and methane as carbon sources produce tungsten carbide nanopowder materials which mostly have complex tungsten and carbon compound components.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention belongs to the field of inorganic nano material preparation and energy conversion and utilization, and particularly relates to a tungsten carbide nano array material prepared by a hydrothermal method and a volatile solid gas-phase chemical deposition method.
The invention relates to a tungsten carbide nano array material, which is characterized by comprising a substrate material and a tungsten carbide nano array structure material grown on the substrate material. The array is an organized arrangement of units with similar structures.
The tungsten carbide nano array structure material can be doped with nitrogen or not. When the material is a nitrogen-doped tungsten carbide nano array structure material, the nitrogen element generally accounts for 0.01-20 wt% of the tungsten carbide nano array structure material.
Preferably, the substrate material can be used as long as the substrate material is stable in a synthetic environment, and the substrate material is one or more of metal, quartz glass, silicon, ceramic or carbon materials.
Preferably, the tungsten carbide nano array structure material only has characteristic peaks of a substrate, carbon and tungsten carbide in an XRD (X-ray diffraction) pattern, and the nitrogen-doped tungsten carbide nano array structure material also only has characteristic peaks of a substrate, carbon and tungsten carbide.
Preferably, the tungsten carbide nanoarray comprises a nanowire array, a nanobelt array, a nanocolumnar array or a nanobweb array.
The second aspect of the invention relates to a preparation method of a tungsten carbide nano array material, which comprises the following steps:
(1) adding a pH regulator and a morphology regulator into the tungsten-containing solution, then adding a substrate material, keeping the temperature at 120-200 ℃ for 0.5-20 h, and cooling to obtain the tungsten oxide nano array material.
(2) And (2) keeping the tungsten oxide nano array material obtained in the step (1) and a carbon source together at 800-950 ℃ for 0.5-3 h under the condition of inert gas to obtain the tungsten carbide nano array material.
In a preferred embodiment of the second aspect of the present invention, the tungsten-containing solution in step (1) is one or more of a tungstic acid solution, an ammonium tungstate solution, a sodium tungstate solution and a tungsten chloride solution.
Preferably, the pH regulator is one or more of acid, alkali, salt and oxide, and may be, but is not limited to, one or more of sulfuric acid, hydrochloric acid, phosphoric acid, sodium hydroxide and potassium hydroxide. The shape regulator is various salts which are easily dissolved in corresponding solutions and cannot be precipitated in the reaction process, and can be one or more of sodium sulfate, potassium sulfate, sodium chloride, potassium chloride, ammonium sulfate or ammonium chloride.
Preferably, the substrate material in step (1) is one or more of metal, quartz glass, silicon, ceramic or carbon material.
Preferably, the carbon source in step (2) is one or more of melamine, dicyandiamide and terpenes, and the terpenes are one or more of camphor, myrcene and citral. As the carbon source of the present invention, as long as the solid powder has thermal volatility and contains elements such as carbon and oxygen, hydrogen, etc.; when the carbon source contains nitrogen elements, a small amount of nitrogen is doped in the tungsten carbide nano array material, but the phase type of tungsten carbide is not influenced.
The third aspect of the invention relates to the application of the tungsten carbide nano array material in photothermal evaporation of water (such as salt water desalination and sewage treatment) or electrocatalytic hydrogen evolution or electrocatalytic oxygen evolution under acidic conditions.
The invention has the beneficial effects that:
(1) the tungsten carbide nano array material has novel appearance and is disclosed for the first time. Tungsten carbide has good light absorption properties. This is related to the subtractive effects of the nanoarray structure, the light absorbing properties of tungsten carbide itself and the plasmon resonance effect. The light absorption performance of the tungsten carbide nano array material is more than 98% in the whole solar spectrum range. The spectral absorption of the tungsten carbide nanoarray material of the present invention is compared with that of nanographite as shown in fig. 12.
(2) The tungsten carbide nano array material adopts the volatile solid as the carbon source, and the safety is improved compared with a tungsten carbide synthesis method using hydrogen and methane as the carbon source. When the carbon source contains nitrogen elements, the tungsten carbide nano array material doped with nitrogen can be obtained, and the nitrogen doping does not influence the pure phase property of the tungsten carbide nano array material.
(3) The tungsten carbide nano array material, particularly nitrogen-doped tungsten carbide nano array material, is used as a catalyst for electrocatalytic hydrogen and oxygen evolution under an acidic condition, and has excellent performance. The cost is low compared with noble metals, and the catalyst is efficient and stable compared with non-noble metals.
(4) The tungsten carbide nano array material can be used for hydrogen production, acid-containing waste liquid treatment and photo-thermal evaporation of water such as salt water desalination, sewage treatment and the like, and is efficient, stable and excellent in performance.
Drawings
FIG. 1 is a scanning electron microscope photomicrograph of a tungsten carbide nanowire array of the present invention;
FIG. 2 is a scanning electron micrograph of an array of tungsten carbide nanoribbons of the present invention;
FIG. 3 is a scanning electron microscope photograph of a tungsten carbide nanopillar array of the present invention;
FIG. 4 is a scanning electron micrograph of a tungsten carbide nano-web array of the present invention;
FIG. 5 is an XRD spectrum of a carbon fiber paper-based tungsten carbide nanoarray according to the present invention;
FIG. 6 is a scanning electron micrograph of an array of tungsten oxide nanoribbons of the present invention;
FIG. 7 is a HER linear scan polarization curve of tungsten carbide nanoarray materials of the invention compared to platinum carbon;
FIG. 8 shows that the tungsten carbide nano-array material of the present invention catalyzes HER at a current density of 20mA cm-2And 50mA cm-2Stability test curve of (1);
FIG. 9 shows that the tungsten carbide nano-array material of the present invention catalyzes HER at a current density of 60mA cm-2Stability test ofA curve;
FIG. 10 shows that the tungsten carbide nano-array material of the present invention catalyzes HER at a current density of 100mA cm-2Stability test curve of (1);
FIG. 11 is an OER polarization curve of tungsten carbide nanoarray materials of the present invention compared to iridium oxide and iridium carbon catalysts;
FIG. 12 is a graph comparing the spectral absorption of a tungsten carbide nanoarray material of the present invention with that of nanographite;
FIG. 13 is a graph comparing the water evaporation rate curves of the tungsten carbide nanoarray material of the present invention with the water evaporation rate curves of the surface of nanographite and the water evaporation rate curves of the surface of water;
FIG. 14 is a graph showing the ion concentration comparison between the tungsten carbide nano-array material before and after the photothermal evaporation treatment of seawater and sewage.
Detailed Description
The present invention is further described below with reference to examples. It should be noted that the examples are not intended to limit the scope of the present invention, and those skilled in the art will appreciate that any modifications and variations based on the present invention are within the scope of the present invention.
The chemical reagents used in the following examples are conventional and are commercially available. The substrate material of this embodiment is carbon fiber paper, and other substrate materials such as metal, quartz glass, silicon, ceramic, etc. can be used to obtain the same effect.
Example 1
0.6g of sodium tungstate was dissolved in 20ml of water to form a homogeneous solution. Then, 100 μ l of sulfuric acid and 0.2g of anhydrous sodium sulfate are added into the solution and mixed evenly, the mixture is put into a polytetrafluoroethylene inner container of a reaction kettle, a carbon fiber paper substrate is added into the polytetrafluoroethylene inner container, the inner container is sealed, the reaction kettle is sealed, hydrothermal reaction is carried out for 18 hours at 200 ℃, and then the sample is cooled and taken out. And obtaining the carbon fiber paper substrate tungsten oxide nano array material.
Putting 2g of camphor and the carbon fiber paper substrate tungsten oxide nano array material into a tubular furnace, introducing argon for protection, reacting for 2 hours at 950 ℃, naturally cooling and taking out a sample. Obtaining the tungsten carbide nanowire array material as shown in figure 1.
Fig. 5 is an XRD spectrum of a tungsten carbide nanoarray based on carbon fiber paper. As can be seen from the graph, only the characteristic peak of the substrate carbon fiber paper, the characteristic peak of the carbon and the characteristic peak of the WC.
Example 2
0.5g of tungsten chloride was dissolved in 20ml of water to obtain a homogeneous solution. Then, 115 mul hydrochloric acid and 0.2g potassium chloride are added into the solution and mixed evenly, the mixture is put into a polytetrafluoroethylene inner container of a reaction kettle, a carbon fiber paper substrate is added into the polytetrafluoroethylene inner container, the inner container is sealed, the reaction kettle is reacted for 12 hours at 180 ℃, and then the sample is cooled and taken out. The carbon fiber paper substrate tungsten oxide nano array material is obtained, and a scanning electron microscope of the obtained sample is shown in figure 6.
Putting 2g of melamine into a tube furnace, putting the carbon fiber paper substrate tungsten oxide nano array material into the tube furnace, introducing argon for protection, reacting for 3 hours at 850 ℃, naturally cooling and taking out a sample. Obtaining the tungsten carbide nano-belt array material as shown in figure 2. The obtained material is a nitrogen-doped tungsten carbide nano array material.
Example 3
0.9g of potassium tungstate was dissolved in 20ml of water to form a homogeneous solution. Then, 200 mul hydrochloric acid and 0.2g potassium sulfate are added into the solution and mixed evenly, the mixture is put into a polytetrafluoroethylene inner container of a reaction kettle, a carbon fiber paper substrate is added into the polytetrafluoroethylene inner container, the inner container is sealed, the reaction kettle is reacted for 12 hours at 180 ℃, and then the sample is cooled and taken out. And obtaining the carbon fiber paper substrate tungsten oxide nano array material.
Placing 2g of dicyandiamide and the carbon fiber paper substrate tungsten oxide nano array material in a tubular furnace, introducing argon for protection, reacting for 1 hour at 800 ℃, naturally cooling and taking out a sample. Obtaining the tungsten carbide nano columnar array material as shown in figure 3. The obtained material is a nitrogen-doped tungsten carbide nano array material.
Example 4
0.3g of sodium tungstate was dissolved in 20ml of water to form a homogeneous solution. Then, 100 mul phosphoric acid and 0.1g sodium chloride are added into the solution and mixed evenly, the mixture is put into a polytetrafluoroethylene inner container of a reaction kettle, a carbon fiber paper substrate is added into the polytetrafluoroethylene inner container, the inner container is sealed, the reaction kettle is sealed, the reaction is carried out for 6 hours at 180 ℃, and then the sample is cooled and taken out. And obtaining the carbon fiber paper substrate tungsten oxide nano array material.
Placing 2g of dicyandiamide and the carbon fiber paper substrate tungsten oxide nano array material in a tubular furnace, introducing argon for protection, reacting for 2 hours at 850 ℃, naturally cooling and taking out a sample. Obtaining the tungsten carbide nano webbed array material as shown in figure 4. The obtained material is a nitrogen-doped tungsten carbide nano array material.
Example 5
Electrocatalytic Hydrogen Evolution Reaction (HER) test.
A 0.5M sulfuric acid solution was selected as the electrolyte and tested using a standard three-electrode system, where the working electrode was the tungsten carbide nanoarray material of example 2, the auxiliary electrode was a carbon rod, and the reference electrode was a silver/silver chloride reference electrode. When the current density is 10mA cm respectively-2、200mA cm-2The overpotentials were only 89mV and 190mV (as shown in FIG. 7), respectively, indicating the high efficiency of the material.
When the current density is respectively 20mA cm-2、50mA cm-2(as shown in FIG. 8), 60mA cm-2(as shown in FIG. 9), 100mA cm-2(as shown in FIG. 10), the current density changes were + 2.9%, -1.9%, -0.5%, and + 1.1% for 10 hours of operation, indicating that the stability of the material was high.
Example 6
Electrocatalytic Oxygen Evolution Reaction (OER) test.
A 0.5M sulfuric acid solution was selected as the electrolyte and tested using a standard three-electrode system, where the working electrode was the tungsten carbide nanoarray material in example 3, the auxiliary electrode was a platinum electrode, and the reference electrode was a silver/silver chloride reference electrode. The initial peak potential is about 1.4V vs. RHE, and when the potential reaches 1.7V vs. RHE, the current density can reach 60mA cm-2(as shown in fig. 11). Illustrating that the tungsten carbide nano-array material in example 3 has a high degree of crystallinity under acidic conditionsEffective OER performance.
Example 7
The laboratory tests the water evaporation rate.
A device for testing the water evaporation rate in a laboratory is used, the light source is a xenon lamp light source, and the illumination condition is AM1.5, namely the illumination condition of the common atmospheric environment. The rate curve of the tungsten carbide nano web array material in example 4 compared with the nano graphite surface water evaporation and the water surface evaporation attack is shown in fig. 13. As can be seen from fig. 13, the water evaporation rate of the surface of the tungsten carbide nano array is 1.25 times that of the surface of nano graphite, and is 1.89 times that of the common water surface. Therefore, the tungsten carbide nano array material can effectively promote the evaporation of water.
Example 8
The tungsten carbide nano array material is used for salt water desalination and sewage treatment.
A device for purifying brine using laboratory water evaporation. The salt water and the sewage are stored in a water storage tank, and can be supplemented through a water inlet, and the liquid level height is controlled through a water outlet, so that the salt water and the distilled water are not mixed. The filter paper absorbs the saline water to the lower surface of the tungsten carbide nano array (the tungsten carbide nano webbed array material obtained in the embodiment 4) through capillary force, the saline water enters the tungsten carbide nano array, under the illumination condition, the tungsten carbide nano array can generate higher temperature, the saline water is evaporated on the surface of the tungsten carbide nano array, the steam is condensed on the condensation cover, and the condensed distilled water can flow into the distilled water collecting tank and is stored in the lower half part of the distilled water collecting tank with lower temperature.
The water quality conditions before and after artificial synthesis of seawater and artificial synthesis of heavy metal ion wastewater are shown in FIG. 14. As can be seen from FIG. 14, the contents of sodium ion, magnesium ion, potassium ion and calcium ion in the artificially synthesized seawater before treatment were 10000ppm, 1000ppm, 120ppm and 130ppm, respectively, and the concentrations of sodium ion, magnesium ion, potassium ion and calcium ion in the treated seawater were 0.6ppm, 0.2ppm, 0.05ppm and 0.1ppm, respectively, which were all reduced to less than 1 ppm. The contents of heavy metal arsenic, cadmium and lead in the sewage polluted by heavy metal before treatment are respectively 1000ppb, 2000ppb and 1700ppb which are respectively about 100 times, 400 times and 110 times of the American first-level drinking water standard, and after treatment, the concentrations of arsenic, cadmium and lead are all reduced to be below the American first-level drinking water standard and are respectively 0.01ppb, 0.17ppb and 0.5ppb, namely the requirements of the drinking water standard are completely met.
Claims (6)
1. The tungsten carbide nano array material is characterized by comprising a substrate material and a tungsten carbide nano array structure material grown on the substrate material; the tungsten carbide nano array structure material only has a characteristic peak of a substrate, a characteristic peak of carbon and a characteristic peak of tungsten carbide in an XRD (X-ray diffraction) pattern; the substrate material is carbon fiber paper.
2. The tungsten carbide nanoarray material of claim 1, wherein the tungsten carbide nanoarray structure material is nitrogen-doped or non-nitrogen-doped.
3. The tungsten carbide nanoarray material of claim 1 or 2, wherein the tungsten carbide nanoarray comprises a nanowire array, a nanoribbon array, a nanocolumnar array, or a nanoweb array.
4. A preparation method of a tungsten carbide nano array material is characterized by comprising the following steps:
(1) adding a pH regulator and a morphology regulator into a tungsten-containing solution, then adding a substrate material, carrying out hydrothermal reaction in a closed container at 120-200 ℃ for 0.5-20 h, and cooling to obtain a tungsten oxide nano array material; the tungsten-containing solution is one or more of tungstic acid solution, ammonium tungstate solution, sodium tungstate solution and tungsten chloride solution; the substrate material is carbon fiber paper;
(2) keeping the tungsten oxide nano array material obtained in the step (1) and a carbon source together at 800-950 ℃ for 0.5-3 h under the condition of inert gas to obtain the tungsten carbide nano array material; the carbon source is one or more of melamine, dicyandiamide and terpenes, and the terpenes are one or more of camphor, myrcene and citral.
5. The preparation method according to claim 4, wherein the pH regulator in step (1) is one or more of acid, alkali, salt and oxide; the shape regulator is one or more of sodium sulfate, potassium sulfate, sodium chloride, potassium chloride, ammonium sulfate or ammonium chloride.
6. Use of the tungsten carbide nanoarray material according to claim 1 or 2 for photothermal evaporation of water or electrocatalytic hydrogen or oxygen evolution under acidic conditions.
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| CN111151293B (en) * | 2019-12-27 | 2023-01-31 | 浙江师范大学 | Nitrogen-doped tungsten carbide catalyst, and preparation and application thereof |
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