CN107999102B - Preparation and performance test of plasma enhanced HER catalyst - Google Patents
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Abstract
The invention discloses a preparation and performance test method of a plasma enhanced HER high-efficiency catalyst, which comprises the following steps: first step, Fe3O4Synthesizing microspheres; second step, synthesis of Fe3O4Au/MOF-based phosphatized nanoparticles. The preparation and performance test of the plasma enhanced HER high-efficiency catalyst have the beneficial effects that: the high-efficiency HER catalyst for enhancing HER by plasma is prepared, so that the supply requirement of platinum metal is greatly relieved, the manufacturing cost is low, and the recycling is facilitated.
Description
Technical Field
The invention relates to the technical field of new energy materials, in particular to preparation and performance test of a plasma enhanced HER catalyst.
Background
A substance that can change (increase or decrease) the chemical reaction rate of a reactant in a chemical reaction without changing the chemical equilibrium and whose own mass and chemical properties are not changed before and after the chemical reaction is called a catalyst (solid catalyst is also called a catalyst). According to statistics, about more than 90% of industrial processes use catalysts, such as chemical industry, petrochemical industry, biochemical industry, environmental protection and the like.
The platinum catalyst is a generic name of a catalyst prepared by taking metal platinum as a main active component. Platinum metal mesh, platinum black, or platinum supported on a carrier such as alumina, and optionally a promoter component such as rhenium. The platinum catalyst is a catalyst commonly used in Hydrogen Evolution Reaction (HER), and because the platinum catalyst is used for manufacturing, platinum metal resources are scarce, and the platinum metal resources are difficult to recycle, the invention of the Hydrogen Evolution Reaction (HER) catalyst which is low in manufacturing cost and beneficial to recycling becomes very important.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the preparation and performance test of the plasma enhanced HER catalyst, and solves the problems that the platinum catalyst is a commonly used catalyst in Hydrogen Evolution Reaction (HER), the preparation cost is high, the platinum metal resource is scarce, and the recycling is difficult.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
preparation and performance test of a plasma enhanced HER catalyst comprise the following steps:
first step, Fe3O4Microsphere synthesis
S1: mixing Fe3O4·6H2Dissolving O (1.35g, 5mmol) in ethylene glycol (40ml) solution to form a uniform solution, and adding NaAc (3.6g) and polyvinylidene (1.0 g);
s2: stirring the mixture for 30 minutes, sealing in an autoclave (50ml) with polytetrafluoroethylene as an inner liner, heating to 200 ℃ and keeping for 9 hours, and then naturally cooling;
s3: washing the black product with ethanol for three times and then drying;
second step, synthesis of Fe3O4Au/MOF-based phosphatized nanoparticles
S1: 20mg of Fe3O4Pretreatment with HCl (5ml, 1M) and sonication for 5 min;
s2: using a magnet to adsorb a sample, and cleaning the sample with ultrapure water for three times;
s3: mixing the product with 20ml of ultrapure water and cysteine aqueous solution (10ml, 10g/L), and ultrasonically treating for 1 hour by using an ultrasonic generator;
s4: separating the sample in the solution by using a magnet, washing the sample by using ultrapure water for three times, and separating the sample into 20ml of ultrapure water again;
s5: 2ml of chloroauric acid (25mM) was added dropwise to the above solution, and stirred for three hours;
s6: 5ml ascorbic acid (1 wt%) was added and stirred for three hours;
s7: separating the product by using a magnet, respectively washing the product by using ultrapure water and ethanol for three times, and dispersing a sample into the ethanol;
s8: the sample was immersed in 4ml FeCl in a 70 ℃ water bath3Ethanol solution (10mM) for 15 minutes, followed by three ethanol washes;
s9: adding 4ml of H under the condition of 70 ℃ water bath3BTC ethanol solution (10mM) and left for 30 minutes, followed by three washes with ethanol solution;
s10: repeating the steps S8-S9, wherein the repetition times can be determined by self;
s11: drying at 120 deg.C under vacuum;
s12: uniformly spreading the sample, placing the sample in a magnetic boat, heating the sample for 2 hours at the high temperature of 900 ℃ by using a tube furnace, and then naturally cooling the sample;
s13: take 0.1gKH2PO4Placing the sample in a magnetic boat at the upper air inlet of the tube furnace, placing the sample in the magnetic boat at the lower air inlet of the tube furnace, and finally obtaining Fe as the catalyst3O4AuFe2PC-9。
Preferably, the method uses a three-electrode system, and uses an electrochemical workstation at 0.5mol/L H2SO4The sweep rate of the electrolyte is 2mV/s, the electrocatalyst has excellent catalytic activity and stability and relatively small resistivity, and the photoelectricity coupling is adopted under the condition of illumination to enhance the HER catalytic performance.
Preferably, in the step of S10, the number of times of repeating the steps of S8 to S9 is 3 to 5.
(III) advantageous effects
The invention provides a preparation and performance test method of a plasma enhanced HER catalyst, which has the following beneficial effects: the HER catalyst for enhancing HER through the plasma is prepared, the supply requirement of platinum metal is greatly relieved, the manufacturing cost is low, and the recycling is facilitated.
Drawings
FIG. 1 shows the present inventionMing Fe3O4a/Au/MOF nanoparticle structure schematic diagram;
FIG. 2 is a schematic diagram of electrocatalytic activity parameters of the present invention, wherein Onstetoverpotential is the initial potential of the sample before and after illumination, η a is before illumination, η b is after illumination, Tafelslope is the slope of the Tafel curve, and Tafelregion is the Tafel selection range;
FIG. 3 shows Fe of the present invention3O4/Au/Fe2P/C-4、Fe3O4/Au/Fe2P/C-14 and polarization curves after illumination thereof [ a ]]Before representing illumination, [ b ]]After representing illumination;
FIG. 4 is a graph of the present invention and Fe3O4/Au/Fe2O3C-9 and polarization curve after illumination [ a ]]Before representing illumination, [ b ]]After representing illumination;
FIG. 5 is a schematic representation of the stability test of a sample of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution:
preparation and performance test of a plasma enhanced HER catalyst comprise the following steps:
first step, Fe3O4Microsphere synthesis
S1: mixing Fe3O4·6H2Dissolving O (1.35g, 5mmol) in ethylene glycol (40ml) solution to form a uniform solution, and adding NaAc (3.6g) and polyvinylidene (1.0 g);
s2: stirring the mixture for 30 minutes, sealing in an autoclave (50ml) with polytetrafluoroethylene as an inner liner, heating to 200 ℃ and keeping for 9 hours, and then naturally cooling;
s3: washing the black product with ethanol for three times and then drying;
second step, synthesis of Fe3O4Au/MOF-based phosphatized nanoparticles
S1: 20mg of Fe3O4Pretreatment with HCl (5ml, 1M) and sonication for 5 min;
s2: using a magnet to adsorb a sample, and cleaning the sample with ultrapure water for three times;
s3: mixing the product with 20ml of ultrapure water and cysteine aqueous solution (10ml, 10g/L), and ultrasonically treating for 1 hour by using an ultrasonic generator;
s4: separating the sample in the solution by using a magnet, washing the sample by using ultrapure water for three times, and separating the sample into 20ml of ultrapure water again;
s5: 2ml of chloroauric acid (25mM) was added dropwise to the above solution, and stirred for three hours;
s6: 5ml ascorbic acid (1 wt%) was added and stirred for three hours;
s7: separating the product by using a magnet, respectively washing the product by using ultrapure water and ethanol for three times, and dispersing a sample into the ethanol;
s8: the sample was immersed in 4ml FeCl in a 70 ℃ water bath3Ethanol solution (10mM) for 15 minutes, followed by three ethanol washes;
s9: adding 4ml of H under the condition of 70 ℃ water bath3BTC ethanol solution (10mM) and left for 30 minutes, followed by three washes with ethanol solution;
s10: repeating the steps S8-S9 for 3-5 times;
s11: drying at 120 deg.C under vacuum;
s12: uniformly spreading the sample, placing the sample in a magnetic boat, heating the sample for 2 hours at the high temperature of 900 ℃ by using a tube furnace, and then naturally cooling the sample;
s13: take 0.1gKH2PO4Placing the sample in a magnetic boat at the upper air inlet of the tube furnace, placing the sample in the magnetic boat at the lower air inlet of the tube furnace, and finally obtaining Fe as the catalyst3O4AuFe2PC-9。
Synthesis of 282nm Fe3O4Nano meterParticles, on the surface of which Au nanoparticles are grown, followed by the growth of MOF thereon, followed by the phosphating thereof, because the thickness of the Au nanoparticles is small and difficult to find in TEM images, but the thickness of the MOF and the middle Fe can be clearly seen3O4And (3) nanoparticles.
Referring to fig. 2: using a three-electrode system, using an electrochemical workstation, at 0.5mol/L H2SO4The sweep rate of the electrolyte of (1) is 2mV/s, which means that the sample is subjected to MOF post-phosphorization for 9 times, Fe3O4/Au/Fe2P/C-4 is expressed as the result of 4 MOF post-phosphatization of the sample, Fe3O4/Au/Fe2P/C-14 is expressed as the result of subjecting the sample to MOF post-phosphating for 14 times, Fe3O4/Au/Fe2O3the/C-9 shows that the sample is not phosphorized after being subjected to MOF for 9 times, the electrocatalyst has excellent catalytic activity and stability, the resistivity is relatively small, and the HER catalytic performance is enhanced by photoelectric coupling under the condition of illumination.
Example one
Referring to fig. 3, a method for preparing a plasma enhanced HER catalyst and testing the performance of the plasma enhanced HER catalyst comprises the following steps:
first step, Fe3O4Microsphere synthesis
S1: mixing Fe3O4·6H2Dissolving O (1.35g, 5mmol) in ethylene glycol (40ml) solution to form a uniform solution, and adding NaAc (3.6g) and polyvinylidene (1.0 g);
s2: stirring the mixture for 30 minutes, sealing in an autoclave (50ml) with polytetrafluoroethylene as an inner liner, heating to 200 ℃ and keeping for 9 hours, and then naturally cooling;
s3: washing the black product with ethanol for three times and then drying;
second step, synthesis of Fe3O4Au/MOF-based phosphatized nanoparticles
S1: 20mg of Fe3O4Pretreatment with HCl (5ml, 1M) and sonication for 5 min;
s2: using a magnet to adsorb a sample, and cleaning the sample with ultrapure water for three times;
s3: mixing the product with 20ml of ultrapure water and cysteine aqueous solution (10ml, 10g/L), and ultrasonically treating for 1 hour by using an ultrasonic generator;
s4: separating the sample in the solution by using a magnet, washing the sample by using ultrapure water for three times, and separating the sample into 20ml of ultrapure water again;
s5: 2ml of chloroauric acid (25mM) was added dropwise to the above solution, and stirred for three hours;
s6: 5ml ascorbic acid (1 wt%) was added and stirred for three hours;
s7: separating the product by using a magnet, respectively washing the product by using ultrapure water and ethanol for three times, and dispersing a sample into the ethanol;
s8: the sample was immersed in 4ml FeCl in a 70 ℃ water bath3Ethanol solution (10mM) for 15 minutes, followed by three ethanol washes;
s9: adding 4ml of H under the condition of 70 ℃ water bath3BTC ethanol solution (10mM) and left for 30 minutes, followed by three washes with ethanol solution;
s10: repeating the steps S8-S9 for 4 times;
s11: drying at 120 deg.C under vacuum;
s12: uniformly spreading the sample, placing the sample in a magnetic boat, heating the sample for 2 hours at the high temperature of 900 ℃ by using a tube furnace, and then naturally cooling the sample;
s13: take 0.1gKH2PO4Placing the sample in a magnetic boat at the upper air inlet of the tube furnace, placing the sample in the magnetic boat at the lower air inlet of the tube furnace, and finally obtaining Fe as the catalyst3O4AuFe2PC-4。
In summary, the following results can be obtained: fe3O4/Au/Fe2P/C-4 is expressed as the result of 4 MOF post-phosphatization of the sample, Fe3O4/Au/Fe2P/C-14 is expressed as the result of subjecting the sample to MOF post-phosphating for 14 times, Fe3O4/Au/Fe2O3the/C-9 shows that the MOF of the sample is not phosphorized after being subjected to MOF for 9 times, the catalytic performance of the three catalysts is enhanced under the illumination condition, and the MOF phosphorization for 9 times is better than that of other samples under the same condition.
Example two
Referring to fig. 4, a method for preparing a plasma enhanced HER catalyst and testing the performance of the plasma enhanced HER catalyst includes the following steps:
first step, Fe3O4Microsphere synthesis
S1: mixing Fe3O4·6H2Dissolving O (1.35g, 5mmol) in ethylene glycol (40ml) solution to form a uniform solution, and adding NaAc (3.6g) and polyvinylidene (1.0 g);
s2: stirring the mixture for 30 minutes, sealing in an autoclave (50ml) with polytetrafluoroethylene as an inner liner, heating to 200 ℃ and keeping for 9 hours, and then naturally cooling;
s3: washing the black product with ethanol for three times and then drying;
second step, synthesis of Fe3O4Au/MOF-based phosphatized nanoparticles
S1: 20mg of Fe3O4Pretreatment with HCI (5ml, 1M) and sonication for 5 min;
s2: using a magnet to adsorb a sample, and cleaning the sample with ultrapure water for three times;
s3: mixing the product with 20ml of ultrapure water and cysteine aqueous solution (10ml, 10g/L), and ultrasonically treating for 1 hour by using an ultrasonic generator;
s4: separating the sample in the solution by using a magnet, washing the sample by using ultrapure water for three times, and separating the sample into 20ml of ultrapure water again;
s5: 2ml of chloroauric acid (25mM) was added dropwise to the above solution, and stirred for three hours;
s6: 5ml ascorbic acid (1 wt%) was added and stirred for three hours;
s7: separating the product by using a magnet, respectively washing the product by using ultrapure water and ethanol for three times, and dispersing a sample into the ethanol;
s8: the sample was immersed in 4ml FeCl in a 70 ℃ water bath3Ethanol solution (10mM) for 15 minutes, followed by three ethanol washes;
s9: adding 4ml of H under the condition of 70 ℃ water bath3BTC ethanol solution (10mM) and left for 30 minutes, followed by three washes with ethanol solution;
s10: repeating the steps S8-S9 for 9 times;
s11: drying at 120 deg.C under vacuum;
s12: uniformly spreading the sample, placing the sample in a magnetic boat, heating the sample for 2 hours at the high temperature of 900 ℃ by using a tube furnace, and then naturally cooling the sample;
s13: take 0.1gKH2PO4Placing the sample in a magnetic boat at the upper air inlet of the tube furnace, placing the sample in the magnetic boat at the lower air inlet of the tube furnace, and finally obtaining Fe as the catalyst3O4AuFe2PC-9。
In summary, the following results can be obtained: fe3O4/Au/Fe2P/C-4 is expressed as the result of 4 MOF post-phosphatization of the sample, Fe3O4/Au/Fe2P/C-14 is expressed as the result of subjecting the sample to MOF post-phosphating for 14 times, Fe3O4/Au/Fe2O3the/C-9 shows that the MOF of the sample is not phosphorized after 9 times of MOF, the catalytic activity of the catalyst is enhanced under the same illumination condition, and the catalytic effect of the MOF phosphorization of 9 times is better than that of the MOF non-phosphorization of 9 times under the same condition.
EXAMPLE III
Referring to fig. 5, a method for preparing a plasma enhanced HER catalyst and testing the performance of the plasma enhanced HER catalyst includes the following steps:
first step, Fe3O4Microsphere synthesis
S1: mixing Fe3O4·6H2Dissolving O (1.35g, 5mmol) in ethylene glycol (40ml) solution to form a uniform solution, and adding NaAc (3.6g) and polyvinylidene (1.0 g);
s2: stirring the mixture for 30 minutes, sealing in an autoclave (50ml) with polytetrafluoroethylene as an inner liner, heating to 200 ℃ and keeping for 9 hours, and then naturally cooling;
s3: washing the black product with ethanol for three times and then drying;
second step, synthesis of Fe3O4Au/MOF-based phosphatized nanoparticles
S1: 20mg of Fe3O4Pretreatment with HCl (5ml, 1M) and sonication for 5 min;
s2: using a magnet to adsorb a sample, and cleaning the sample with ultrapure water for three times;
s3: mixing the product with 20ml of ultrapure water and cysteine aqueous solution (10ml, 10g/L), and ultrasonically treating for 1 hour by using an ultrasonic generator;
s4: separating the sample in the solution by using a magnet, washing the sample by using ultrapure water for three times, and separating the sample into 20ml of ultrapure water again;
s5: 2ml of chloroauric acid (25mM) was added dropwise to the above solution, and stirred for three hours;
s6: 5ml ascorbic acid (1 wt%) was added and stirred for three hours;
s7: separating the product by using a magnet, respectively washing the product by using ultrapure water and ethanol for three times, and dispersing a sample into the ethanol;
s8: the sample was immersed in 4ml FeCl in a 70 ℃ water bath3Ethanol solution (10mM) for 15 minutes, followed by three ethanol washes;
s9: adding 4ml of H under the condition of 70 ℃ water bath3BTC ethanol solution (10mM) and left for 30 minutes, followed by three washes with ethanol solution;
s10: repeating the steps S8-S9 for 14 times;
s11: drying at 120 deg.C under vacuum;
s12: uniformly spreading the sample, placing the sample in a magnetic boat, heating the sample for 2 hours at the high temperature of 900 ℃ by using a tube furnace, and then naturally cooling the sample;
s13: take 0.1gKH2PO4Placing the sample in a magnetic boat at the upper air inlet of the tube furnace, placing the sample in the magnetic boat at the lower air inlet of the tube furnace, and finally obtaining Fe as the catalyst3O4AuFe2PC-14。
In summary, the following results can be obtained: it can be seen that the catalytic activity of the sample was not substantially changed before 1000 cycles and after 1000 cycles, indicating that the catalytic stability of the sample was good.
In summary, the following steps: the invention provides a preparation and performance test method of a plasma enhanced HER catalyst, which has the following beneficial effects: the HER catalyst for enhancing HER through the plasma is prepared, the supply requirement of platinum metal is greatly relieved, the manufacturing cost is low, and the recycling is facilitated.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. A method for preparing a plasma-enhanced HER high-efficiency catalyst, which is characterized by comprising the following steps: the method comprises the following steps:
first step, Fe3O4Microsphere synthesis
S1: 1.35g, 5mmol of Fe3O4·6H2Dissolving O in 40mL of glycol solution to form a uniform solution, and adding 3.6g of NaAc and 1.0g of polyvinylidene;
s2: stirring the mixture for 30 minutes, sealing the mixture in a 50mL autoclave with polytetrafluoroethylene as an inner liner, heating the mixture to 200 ℃ and keeping the temperature for 9 hours, and then naturally cooling the mixture;
s3: washing the black product with ethanol for three times and then drying;
second step, synthesis of Fe3O4Au/MOF-based phosphatized nanoparticles
S1: 20mg of Fe3O4Pretreating with 5mL of 1M HCl and performing ultrasonic treatment for 5 minutes;
s2: using a magnet to adsorb a sample, and cleaning the sample with ultrapure water for three times;
s3: fully mixing a sample with 20mL of ultrapure water and 10mL of cysteine aqueous solution with the concentration of 10g/L, and carrying out ultrasonic treatment for 1 hour by using an ultrasonic generator;
s4: separating the sample in the solution by using a magnet, washing the sample by using ultrapure water for three times, and separating the sample into 20mL of ultrapure water again;
s5: 2mL of chloroauric acid with the concentration of 25mM is added into the solution drop by drop, and the solution is stirred for three hours;
s6: then 5mL of ascorbic acid with the concentration of 1 wt% is added, and the mixture is stirred for three hours;
s7: separating the product by using a magnet, respectively washing the product by using ultrapure water and ethanol for three times, and dispersing a sample into the ethanol;
s8: the sample was immersed in 4mL of FeCl with a concentration of 10mM under a water bath condition at 70 deg.C3Standing in ethanol solution for 15 minutes, and then washing with ethanol for three times;
s9: 4mL of 10mM H were added under 70 ℃ water bath condition3BTC ethanol solution and left to stand for 30 minutes, followed by three washes with ethanol solution;
s10: repeating the steps S8-S9, wherein the repetition times can be determined by self;
s11: drying at 120 deg.C under vacuum;
s12: uniformly spreading the sample, placing the sample in a magnetic boat, heating the sample for 2 hours at the high temperature of 900 ℃ by using a tube furnace, and then naturally cooling the sample;
s13: in the heating process in step S12, 0.1g KH was taken2PO4Placing the sample in a magnetic boat at the upper air inlet of the tube furnace, placing the sample in the magnetic boat at the lower air inlet of the tube furnace, and finally obtaining Fe as the catalyst3O4AuFe2PC。
2. Use of the plasma-enhanced HER high-efficiency catalyst prepared by the preparation method of claim 1, wherein the preparation method comprises the following steps: using a three-electrode system, using an electrochemical workstation, at 0.5mol/L H2SO4The sweep rate of the electrolyte is 2mV/s, the electrocatalyst has catalytic activity and stability, and the photoelectricity coupling is realized under the condition of illumination to enhance the HER catalytic performance.
3. The preparation of a plasma-enhanced HER high efficiency catalyst of claim 1, wherein: in the step of S10, the steps of S8-S9 are repeated for 3-5 times.
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