CN108203095A - A kind of tungsten carbide nano-array material, preparation method and the usage - Google Patents
A kind of tungsten carbide nano-array material, preparation method and the usage Download PDFInfo
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- CN108203095A CN108203095A CN201810070110.3A CN201810070110A CN108203095A CN 108203095 A CN108203095 A CN 108203095A CN 201810070110 A CN201810070110 A CN 201810070110A CN 108203095 A CN108203095 A CN 108203095A
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- B01J27/24—Nitrogen compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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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 kind of tungsten carbide nano-array materials, and including base material and the tungsten carbide nano array structure material being grown on base material, the tungsten carbide nano array structure material can be N doping or non-N doping；The tungsten carbide nano array structure includes nano-wire array, nano-band array, nanometer columnar arrays or nanometer web shape array.Preparation method and electrocatalytic hydrogen evolution the invention also discloses the tungsten carbide nano-array material analyse the purposes of oxygen and efficiency light thermal evaporation water purification.
Description
Technical field
The invention belongs to inorganic nano materials to prepare with utilizing field, and in particular to a kind of tungsten carbide nano-array material,
Preparation method and the usage.
Background technology
Tungsten carbide (WC) is cheap, is often used in the preparation of hard metal, and property is stablized.In air, 400 DEG C with
Under be stable.Tungsten carbide has good electric conductivity, thermal conductivity.Research shows that tungsten carbide has plasma resonance effect,
And anti-laser irradiation.Tungsten carbide is very stable in acid system, and has and acted on catalytic hydrogenolysis as platinum class, and this hydrogenolysis is made
With many organic catalysis, electro-catalysis field can be extended to.Above various characteristics so that the research of tungsten carbide material is by wide
General concern, tungsten carbide material is also increasingly being applied to produce, lives and military industry field.
However, the preparation of the nano material of tungsten carbide faces problems at present.Firstth, current tungsten carbide nano material is more
Based on dusty material, however dusty material needs to disperse again in practical applications, is sintered, sprays, and the carbon sprayed
Changing tungsten material cannot be with substrate good contact, these can all be adversely affected in the application, such as after influencing material forming
Specific surface area, hardness, electric conductivity etc..Secondth, the preparation of tungsten carbide is needed by a high temperature cabonization process, this process
Using the gaseous mixture of hydrogen and methane mostly, this causes production process than relatively hazardous as carbon source.Third, not using of having been reported that
Hydrogen and methane have complicated tungsten, carbon compound more as the tungsten carbide nano-powder material that the synthetic method of carbon source is produced
Object ingredient.
To solve the above-mentioned problems, the present invention is proposed.
Invention content
Prepared the invention belongs to inorganic nano material and energy conversion with using field, and in particular to by hydro-thermal method with can
Volatile solids chemical vapor deposition method prepares tungsten carbide nano-array material, and tungsten carbide nano-array material prepared by this method was both
Acid system electrocatalytic hydrogen evolution, electro-catalysis analysis oxygen are can be applied to, is equally applicable at the photo-thermal evaporation such as saline-water reclamation, sewage of water
Reason etc..
First aspect present invention is related to a kind of tungsten carbide nano-array material, which is characterized in that including base material and life
The tungsten carbide nano array structure material being longer than on base material.The array is exactly that the similar unit of structure is systematically arranged
Row.
The tungsten carbide nano array structure material can be N doping or non-N doping.When the tungsten carbide for N doping is received
During rice array structure materials, general nitrogen accounts for 0.01~20wt% of tungsten carbide nano array structure material.
Preferably, as long as the base material stabilization can use in synthetic environment, substrate of the present invention
Material is one or more of metal, quartz glass, silicon, ceramics or carbon material.
Preferably, the tungsten carbide nano array structure material only has the feature of the characteristic peak of substrate, carbon in XRD spectrum
The characteristic peak at peak and tungsten carbide, the tungsten carbide nano array structure material of N doping also only have the feature of the characteristic peak of substrate, carbon
The characteristic peak at peak and tungsten carbide.
Preferably, the tungsten carbide nano-array includes nano-wire array, nano-band array, nanometer columnar arrays or nanometer
Web shape array.
Second aspect of the present invention is related to a kind of preparation method of tungsten carbide nano-array material, includes the following steps：
(1) base material is added after adding in pH adjusting agent and pattern conditioning agent in tungstenic solution, 120 DEG C~200
0.5~20h is kept under the conditions of DEG C, cooling obtains tungsten oxide nanometer array material.
(2) the tungsten oxide nanometer array material for obtaining step (1) is together with carbon source, in 800 DEG C~950 DEG C and indifferent gas
Under the conditions of keep 0.5~3h to be to obtain the tungsten carbide nano-array material.
In the preferred embodiment of the second aspect of the present invention, the tungstenic solution described in step (1) is tungstic acid, tungsten
One or more of acid ammonium solution, sodium tungstate solution, tungsten chloride solution.
Preferably, the pH adjusting agent for acid, alkali, salt, oxide one or more, can be but not limited to sulfuric acid,
One or more of hydrochloric acid, phosphoric acid, sodium hydroxide, potassium hydroxide.The pattern conditioning agent is is soluble in corresponding solution, anti-
The various salts that will not be precipitated out during answering, can be but not limited to sodium sulphate, potassium sulfate, sodium chloride, potassium chloride, sulfuric acid
The one or more of ammonium or ammonium chloride.
Preferably, the base material described in step (1) for one kind in metal, quartz glass, silicon, ceramics or carbon material or
It is several.
Preferably, the carbon source described in step (2) be melamine, dicyandiamide, one or more of terpene, the terpene
For one or more of camphor, laurene, citral.As long as solid powder is first with hot volatility and carbon containing and oxygen, hydrogen etc.
Element can be used as the carbon source of the present invention；When containing nitrogen in carbon source, a small amount of N doping is had in tungsten carbide nano-array material
In material, but the phase type of tungsten carbide is not influenced.
Third aspect present invention is related to the tungsten carbide nano-array material, and for the photo-thermal evaporation of water, (such as brine is light
Change, sewage disposal) or the purposes of oxygen is analysed in electrocatalytic hydrogen evolution or electro-catalysis in acid condition.
Beneficial effects of the present invention：
(1) novel in shape of tungsten carbide nano-array material of the invention is first public.Tungsten carbide has good light
Absorption characteristic.This anti-reflection effect with nano array structure, tungsten carbide optical absorption characteristics in itself and plasma resonance effect
It is related.The absorbing properties of the tungsten carbide nano-array material of the present invention are all higher than 98% in the range of entire solar spectrum.This
The comparison that the spectral absorption of the tungsten carbide nano-array material of invention carries out spectral absorption with nano-graphite is as shown in figure 12.
(2) tungsten carbide nano-array material of the invention using volatilizable solid as carbon source, relative to using hydrogen with
The safety is improved as the tungsten carbide synthetic method of carbon source for methane.When carbon source Nitrogen element, N doping can also be obtained in carbon
Change tungsten nano-array material, and N doping does not influence the property of tungsten carbide nano-array material pure phase completely.
(3) tungsten carbide nano-array material particularly N doping of the invention is used as in tungsten carbide nano-array material in acid
Property under the conditions of electrocatalytic hydrogen evolution analysis oxygen catalyst, have excellent performance.It is at low cost for noble metal, relative to base metal
For efficient stable.
(4) tungsten carbide nano-array material of the invention can be used for the production of hydrogen, the processing containing acid waste liquid, Yi Jiyong
Such as saline-water reclamation, sewage disposal is evaporated in the photo-thermal of water, efficiently, stablizes, has excellent performance.
Description of the drawings
Fig. 1 is the electron scanning micrograph of the tungsten carbide nanowires array of the present invention；
Fig. 2 is the electron scanning micrograph of the tungsten carbide nano-band array of the present invention；
Fig. 3 is the electron scanning micrograph of the tungsten carbide nanometer columnar arrays of the present invention；
Fig. 4 is the electron scanning micrograph of the tungsten carbide nanometer web shape array of the present invention；
Fig. 5 is the XRD spectrum using carbon fiber paper as the tungsten carbide nano-array of substrate of the present invention；
Fig. 6 is electron scanning micrograph of the tungsten oxide nanometer with array of the present invention；
Fig. 7 is the tungsten carbide nano-array material of the present invention and the HER linear scan polarization curves of platinum carbon comparison；
The tungsten carbide nano-array material that Fig. 8 is the present invention is catalyzed HER in current density 20mA cm-2With 50mA cm-2's
Stability test curve；
The tungsten carbide nano-array material that Fig. 9 is the present invention is catalyzed HER in current density 60mA cm-2Stability test
Curve；
The tungsten carbide nano-array material that Figure 10 is the present invention is catalyzed HER in current density 100mA cm-2Stability survey
Try curve；
Figure 11 is that the OER polarization that the tungsten carbide nano-array material of the present invention and yttrium oxide and iridium C catalyst compare is bent
Line；
Figure 12 is that the tungsten carbide nano-array material spectrum of the present invention absorbs the comparison diagram with nano-graphite spectral absorption；
Figure 13 is the tungsten carbide nano-array material water evaporation of the present invention and nano-graphite surface water evaporation and water surface
The rate curve comparison diagram of evaporation；
Figure 14 is the ion concentration pair before and after the tungsten carbide nano-array material photo-thermal evaporation process seawater of the present invention, sewage
Than figure.
Specific embodiment
The present invention is described further with reference to embodiments.It should be noted that embodiment cannot function as to this hair
The limitation of bright protection domain, it will be understood by those skilled in the art that, any improvement and variation made on the basis of the present invention all exist
Within protection scope of the present invention.
Chemical reagent used in following embodiment is all conventional reagent, commercially available.The base material of the present embodiment is equal
For carbon fiber paper, same effect can also be obtained using other base materials such as metal, quartz glass, silicon, ceramics etc..
Embodiment 1
0.6g sodium tungstates is taken to be dissolved in 20ml water, form it into homogeneous solution.Then, 100 μ l sulphur are added in the solution
Acid and 0.2g anhydrous sodium sulfates are uniformly mixed, and are put into the polytetrafluoroethylliner liner of reaction kettle, are added in polytetrafluoroethylliner liner
Carbon fiber paper substrate, sealing inner container seal reaction kettle, then hydro-thermal reaction 18 hours at 200 DEG C cool down and take out sample.
Obtain carbon fiber paper substrate tungsten oxide nanometer array material.
2g camphors are put into tube furnace, are put into above-mentioned carbon fiber paper substrate tungsten oxide nanometer array material, leads to argon gas and protects
Shield is reacted 2 hours at 950 DEG C, and Temperature fall simultaneously takes out sample.Tungsten carbide nanowires array material is obtained, as shown in Figure 1.
Fig. 5 is using carbon fiber paper as the XRD spectrum of the tungsten carbide nano-array of substrate.As can be seen that only from collection of illustrative plates
The characteristic peak of the characteristic peak of substrate carbon fiber paper, the characteristic peak of carbon and WC.
Embodiment 2
0.5g tungsten chlorides is taken to be dissolved in 20ml water, homogeneous solution.Then, 115 μ l hydrochloric acid and 0.2g are added in the solution
Potassium chloride is uniformly mixed, and is put into the polytetrafluoroethylliner liner of reaction kettle, carbon fiber paper substrate is added in polytetrafluoroethylliner liner,
Sealing inner container seals reaction kettle, is reacted 12 hours at 180 DEG C, then cools down and take out sample.Obtain carbon fiber paper substrate oxidation
Tungsten nano-array material, the scanning electron microscope of acquired sample are as shown in Figure 6.
2g melamines are put into tube furnace, are put into above-mentioned carbon fiber paper substrate tungsten oxide nanometer array material, lead to argon
Gas shielded reacts 3 hours at 850 DEG C, and Temperature fall simultaneously takes out sample.Tungsten carbide nano-band array material is obtained, such as Fig. 2 institutes
Show.The present embodiment obtain be N doping tungsten carbide nano-array material.
Embodiment 3
0.9g potassium tungstates is taken to be dissolved in 20ml water, form it into homogeneous solution.Then, 200 μ l salt are added in the solution
Acid and 0.2g potassium sulfates are uniformly mixed, and are put into the polytetrafluoroethylliner liner of reaction kettle, and it is fine that carbon is added in polytetrafluoroethylliner liner
Paper substrates are tieed up, sealing inner container seals reaction kettle, is reacted 12 hours at 180 DEG C, then cools down and take out sample.Obtain carbon fiber
Paper substrates tungsten oxide nanometer array material.
2g dicyandiamides are put into tube furnace, are put into above-mentioned carbon fiber paper substrate tungsten oxide nanometer array material, lead to argon gas
Protection is reacted 1 hour at 800 DEG C, and Temperature fall simultaneously takes out sample.Tungsten carbide nanometer column array material is obtained, such as Fig. 3 institutes
Show.The present embodiment obtain be N doping tungsten carbide nano-array material.
Embodiment 4
0.3g sodium tungstates is taken to be dissolved in 20ml water, form it into homogeneous solution.Then, 100 μ l phosphorus are added in the solution
Acid and 0.1g sodium chloride are uniformly mixed, and are put into the polytetrafluoroethylliner liner of reaction kettle, and it is fine that carbon is added in polytetrafluoroethylliner liner
Paper substrates are tieed up, sealing inner container seals reaction kettle, is reacted 6 hours at 180 DEG C, then cools down and take out sample.Obtain carbon fiber paper
Substrate tungsten oxide nanometer array material.
2g dicyandiamides are put into tube furnace, are put into above-mentioned carbon fiber paper substrate tungsten oxide nanometer array material, lead to argon gas
Protection is reacted 2 hours at 850 DEG C, and Temperature fall simultaneously takes out sample.Tungsten carbide nanometer web shape array material is obtained, such as Fig. 4 institutes
Show.The present embodiment obtain be N doping tungsten carbide nano-array material.
Embodiment 5
Electrocatalytic hydrogen evolution reaction (HER) test.
The sulfuric acid solution of 0.5M is selected to be tested as electrolyte using the three-electrode system of standard, wherein the electricity that works
Tungsten carbide nano-array material extremely in embodiment 2, auxiliary electrode are carbon-point, and reference electrode is silver/silver chloride reference electrode.
When current density is respectively 10mA cm-2、200mA cm-2When, overpotential only be respectively 89mV, 190mV (as shown in Figure 7),
Illustrate the high efficiency of the material.
When current density is respectively 20mA cm-2、50mA cm-2(as shown in Figure 8), 60mA cm-2(as shown in Figure 9),
100mA cm-2During (as shown in Figure 10) left and right, the variable quantity of the current density of work 10 hours is respectively+2.9%, -1.9%, -
0.5% and+1.1%, illustrate that the stability of material is very high.
Embodiment 6
Electro-catalysis oxygen evolution reaction (OER) is tested.
The sulfuric acid solution of 0.5M is selected to be tested as electrolyte using the three-electrode system of standard, wherein the electricity that works
Tungsten carbide nano-array material extremely in embodiment 3, auxiliary electrode are platinum electrode, and reference electrode is silver/silver chloride reference electricity
Pole.It plays spike potential in 1.4V vs.RHE or so, and when current potential reaches 1.7V vs.RHE, current density can reach 60mA
cm-2(as shown in figure 11).Illustrate that the tungsten carbide nano-array material in embodiment 3 has efficient OER in acid condition
Energy.
Embodiment 7
Laboratory test water evaporation rate.
Using the device of laboratory test water evaporation rate, light source used be xenon source, illumination condition AM1.5, i.e.,
Normal atmospheric conditions illumination condition.Using the tungsten carbide nanometer web shape array material in embodiment 4, steamed with nano-graphite surface water
The rate curve that hair, water surface evaporation compare is as shown in figure 13.It can be observed from fig. 13 that tungsten carbide nano-array surface
Water evaporation rate is 1.25 times of nano-graphite surface water evaporation rate, is 1.89 times of light water surface evaporation rate.Therefore
Tungsten carbide nano-array material can effectively facilitate the evaporation of water.
Embodiment 8
Tungsten carbide nano-array material is for saline-water reclamation, sewage disposal.
Use the device of laboratory water evaporation purification brine.Brine and sewage are stored in " aqua storage tank ", and can by into
The mouth of a river is supplemented, controls liquid level by water outlet, and brine and distilled water is made not to mix.Filter paper is by capillary force by brine
Tungsten carbide nano-array (the tungsten carbide nanometer web shape array material that embodiment 4 obtains) lower surface is drawn onto, brine enters tungsten carbide
Nano-array, under illumination condition, tungsten carbide nano-array can generate higher temperature, and brine is in tungsten carbide nano-array table
Face is evaporated, and steam condenses on " condensation lid ", and the distilled water of condensation can flow into " distillation water collecting groove ", and be stored in temperature and compare
The lower half portion of low " distillation water collecting groove ".
Water quality situation before and after artificial synthesized seawater and artificial synthesized heavy metal ion sewage disposal is as shown in figure 14.From figure
As can be seen that before treatment in 14, sodium ion in artificial synthesized seawater, magnesium ion, potassium ion, calcium ion content be respectively
10000ppm, 1000ppm, 120ppm and 130ppm, sodium ion in water, magnesium ion, potassium ion, calcium ion after processing
Concentration is respectively 0.6ppm, 0.2ppm, 0.05ppm and 0.1ppm, all falls below below 1ppm.The sewage of heavy metal pollution is being located
The content of heavy metal arsenic, cadmium, lead before reason is respectively 1000ppb, 2000ppb and 1700ppb, is U.S.'s level-one drinking water respectively
100 times, 400 times and 110 times or so of standard, after processing, arsenic, cadmium, lead concentration be reduced to U.S.'s level-one drinking water
Below the mark, respectively 0.01ppb, 0.17ppb and 0.5ppb fully meet drinking water standard requirement.
Claims (10)
1. a kind of tungsten carbide nano-array material, which is characterized in that including base material and the carbonization being grown on base material
Tungsten nano array structure material.
2. tungsten carbide nano-array material according to claim 1, which is characterized in that the tungsten carbide nano array structure
Material is N doping or non-N doping.
3. tungsten carbide nano-array material according to claim 1 or 2, which is characterized in that the base material for metal,
One or more of quartz glass, silicon, ceramics or carbon material.
4. tungsten carbide nano-array material according to claim 1 or 2, which is characterized in that the tungsten carbide nano-array
Structural material only has characteristic peak, the characteristic peak of carbon and the characteristic peak of tungsten carbide of substrate in XRD spectrum.
5. tungsten carbide nano-array material according to claim 1 or 2, which is characterized in that the tungsten carbide nano-array
Including nano-wire array, nano-band array, nanometer columnar arrays or nanometer web shape array.
6. a kind of preparation method of tungsten carbide nano-array material, which is characterized in that include the following steps：
(1) base material is added after adding in pH adjusting agent and pattern conditioning agent in tungstenic solution, at 120 DEG C~200 DEG C
0.5~20h of hydro-thermal reaction in closed container, cooling obtain tungsten oxide nanometer array material.
(2) the tungsten oxide nanometer array material for obtaining step (1) is together with carbon source, in 800 DEG C~950 DEG C and indifferent gas condition
It is lower that 0.5~3h is kept to obtain the tungsten carbide nano-array material.
7. preparation method according to claim 6, which is characterized in that tungstenic solution described in step (1) is tungstic acid,
One or more of ammonium tungstate solution, sodium tungstate solution, tungsten chloride solution；The base material for metal, quartz glass,
One or more of silicon, ceramics or carbon material.
8. preparation method according to claim 6, which is characterized in that pH adjusting agent described in step (1) is acid, alkali, salt,
One or more of oxide；The pattern conditioning agent is sodium sulphate, potassium sulfate, sodium chloride, potassium chloride, ammonium sulfate or chlorination
One or more of ammonium.
9. preparation method according to claim 6, which is characterized in that the carbon source described in step (2) is melamine, double cyanogen
One or more of amine, terpene, the terpene are one or more of camphor, laurene, citral.
10. tungsten carbide nano-array material according to claim 1 or 2 for water photo-thermal evaporation or in acid condition
The purposes of electrocatalytic hydrogen evolution or electro-catalysis analysis oxygen.
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Cited By (6)
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| CN110676475A (en) * | 2019-08-26 | 2020-01-10 | 广西大学 | Pt-Ni alloy electrocatalyst with layered framework structure and preparation method thereof |
| CN111151293A (en) * | 2019-12-27 | 2020-05-15 | 浙江师范大学 | Nitrogen-doped tungsten carbide catalyst and preparation and application thereof |
| CN111408390A (en) * | 2020-03-12 | 2020-07-14 | 中国科学院上海硅酸盐研究所 | Pure phase polygon W2C nano material and preparation method thereof |
| CN113584520A (en) * | 2021-07-26 | 2021-11-02 | 中国科学院广州能源研究所 | Super-hydrophilic molybdenum-doped tungsten carbide nano array material and preparation method thereof |
| CN113755886A (en) * | 2021-09-09 | 2021-12-07 | 河北大学 | Carbon-coated tungsten nitride and/or tungsten carbide nanowire composite structure and preparation method thereof |
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