CN118112070A - Pt/CrVN2Gas-sensitive electrode material, and preparation method and application thereof - Google Patents
Pt/CrVN2Gas-sensitive electrode material, and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of gas sensors, and particularly relates to a Pt/CrVN 2 gas-sensitive electrode material, and a preparation method and application thereof. The preparation method comprises the following steps: adding deionized water into a chromium source, a vanadium source and urea, and performing ultrasonic treatment to obtain a mixed solution; heating the mixed solution for reaction, centrifugally collecting reactants, and drying in vacuum to obtain CrVN 2 precursor; calcining the CrVN 2 precursor to obtain CrVN 2 material; mixing CrVN 2 the material, glycol and H 2PtCl6 water solution, performing ultrasonic treatment, performing heating reaction, centrifuging, and vacuum drying to obtain the Pt/CrVN 2 gas-sensitive electrode material. The preparation method has the advantages of short reaction time, simple operation and the like; the Pt/CrVN 2 gas-sensitive electrode material has excellent electrochemical performance, and the Pt/CrVN 2 gas-sensitive electrode material has excellent moisture resistance; the gas sensor prepared from the Pt/CrWN 2 gas-sensitive electrode material has excellent long-term stability and quick response recovery performance.
Description
Technical Field
The invention belongs to the technical field of gas sensors, and particularly relates to a Pt/CrVN 2 gas-sensitive electrode material, and a preparation method and application thereof.
Background
The disclosure of this background section is intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
Hydrogen sulfide (H 2 S) is a very important chemical feedstock with a wide range of applications, while H 2 S toxicity is often dependent on its concentration and contact time, since H 2 S is a dangerous toxic gas. When a person is in hydrogen sulfide at a concentration of 10-50 ppm, headache, nausea, eye stinging and the like can be felt, and the symptoms are aggravated by long-term exposure to the environment; when the concentration is between 100 and 500 ppm, the eyes and the respiratory system of the human body can be seriously stimulated, so that the human body is seriously uncomfortable and irreversibly damaged; when the concentration is 500-1000 ppm, the human body can lose consciousness instantaneously, and the human body can die after long-time exposure. When the concentration exceeds 1000 ppm, death is immediately caused. Therefore, the hydrogen sulfide can be monitored rapidly, accurately and stably for a long time, and the threat of the hydrogen sulfide to human health can be effectively avoided.
Conventional (PEM) fuel cell type gas sensors often use porous carbon as a carrier and Pt particles as a catalyst, and the porous carbon is easily corroded and decomposed under electrochemical oxidation conditions to generate carbon oxides, so that the Pt particles are agglomerated, and further, the active sites of Pt are reduced, so that the sensitivity of the sensor is greatly reduced or even disabled. The development of more sensitive, efficient, more stable fuel cell sensors remains a serious challenge.
Disclosure of Invention
Aiming at the defects of the prior art, the first aim of the invention is to provide a preparation method of a Pt/CrVN 2 gas-sensitive electrode material; the preparation method utilizes a hydrothermal-ammonolysis method to jointly prepare CrVN 2, the obtained CrVN 2 sample is loaded with noble metal Pt to synthesize the Pt/CrWN 2 gas-sensitive electrode material, and the preparation method has the advantages of short reaction time, simplicity in operation and the like, and is a simple and efficient preparation method of ternary transition metal nitride.
A second object of the present invention is to provide the Pt/CrVN 2 gas-sensitive electrode material prepared by the above method; the Pt/CrVN 2 gas-sensitive electrode material has excellent moisture resistance.
A third object of the present invention is to provide the use of the above Pt/CrVN 2 gas-sensitive electrode material; the Pt/CrVN 2 gas-sensitive electrode material is used for preparing a hydrogen sulfide gas sensor, and the gas sensor has excellent long-term stability and quick response recovery performance.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
A preparation method of a Pt/CrVN 2 gas-sensitive electrode material comprises the following steps:
(1) Taking a chromium source, a vanadium source and urea, adding deionized water, and performing ultrasonic treatment to obtain a mixed solution;
(2) Heating the mixed solution obtained in the step (1), centrifuging to collect reactants, and drying in vacuum to obtain CrVN 2 precursor;
(3) Calcining the CrVN 2 precursor obtained in the step (2) to obtain CrVN 2 material;
(4) Mixing CrVN 2 material obtained in the step (3), glycol and H 2PtCl6 water solution, performing ultrasonic treatment, and performing heating reaction to obtain a reaction solution;
(5) And (3) centrifuging the reaction liquid obtained in the step (4), and vacuum drying to obtain the Pt/CrVN 2 gas-sensitive electrode material.
Further, in step (1), the chromium source is chromium chloride hexahydrate (CrCl 3·6H2 O) and the vanadium source is vanadium chloride (VCl 3).
Further, in the step (1), the molar volume ratio of the chromium source, the vanadium source, the urea and the deionized water is (1-2) mmol: (1-2) mmol: (2-4) mmol: (25-50) mL; urea functions to provide an alkaline environment.
Further, in the step (1), the time of the ultrasonic treatment is 30-60 min.
Further, in the step (2), the temperature of the heating reaction is 140-180 ℃ and the time is 3-6 h.
Further, in the step (2), the reaction is cooled to room temperature after the heating reaction.
Further, in the step (2), the rotational speed of the centrifugation is 8000-10000 r/min, and the time is 5-10 min.
Further, in step (2), the reactants are collected by centrifugation and then washed.
Further, in the step (2), the temperature of the vacuum drying is 40-60 ℃ and the time is 8-12 h.
Further, in the step (3), the calcination is performed under an ammonia atmosphere at 600-800 ℃ for 6-8 h ℃ and at a heating rate of 3-5 ℃/min.
Further, in the step (3), cooling to room temperature after calcination, and introducing argon gas for 1-1.5; the purpose of the argon is to ensure complete removal of NH 3.
Further, in the step (4), the mass concentration of the H 2PtCl6 aqueous solution is 100 mg/L; the H 2PtCl6 aqueous solution is prepared by the following steps: 1g chloroplatinic acid hydrate was added to a 100 mL volumetric flask and subsequently sized to 100 mL with deionized water.
Further, in the step (4), the mass-to-volume ratio of the CrVN 2 material, the ethylene glycol and the H 2PtCl6 aqueous solution is (5-10) mg: (5-10) mL: (34-68) μl.
Further, in the step (4), the time of the ultrasonic treatment is 30-60 min.
Further, in the step (4), the temperature of the heating reaction is 140-150 ℃ and the time is 3-4 h.
Further, in the step (5), the rotational speed of the centrifugation is 8000-10000 r/min, and the time is 5min.
Further, in the step (5), the temperature of the vacuum drying is 40-60 ℃ and the time is 8-12 h.
The Pt/CrVN 2 gas-sensitive electrode material prepared by the method.
The Pt/CrVN 2 gas-sensitive electrode material is used for preparing a gas sensor.
Further, the gas sensor is used for detecting H 2 S gas.
According to the invention, crVN 2 is prepared by combining a hydrothermal-ammonolysis method, an obtained CrWN 2 sample is prepared by combining the hydrothermal-ammonolysis method, and a noble metal Pt is carried to synthesize the Pt/CrWN 2 gas-sensitive electrode material. The strong interaction between the Transition Metal Nitride (TMNs) and Pt ensures that the electronic structure of Pt atoms is changed, so that the adsorption energy, the reaction activation energy and the electron transfer path of the catalyst carrier to different gases can be predictably changed, and the gas sensor has better sensitivity, selectivity and stability. A step of
The beneficial effects are that: (1) The preparation method utilizes a hydrothermal-ammonolysis method to jointly prepare CrVN 2, and the obtained CrVN 2 material carries noble metal Pt to synthesize Pt/CrVN 2 gas-sensitive electrode material, and has the advantages of short reaction time, simplicity in operation and the like, thus being a simple and efficient preparation method of ternary transition metal nitride.
(2) The Pt/CrVN 2 gas-sensitive electrode material prepared by the scheme of the invention has excellent electrochemical performance, and the Pt/CrVN 2 gas-sensitive electrode material has excellent moisture resistance. The gas sensor prepared from the Pt/CrWN 2 gas-sensitive electrode material has excellent long-term stability and quick response recovery performance.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. Embodiments of the present invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is an XRD pattern for CrVN 2 and Pt/CrVN 2 materials prepared in example 1;
FIG. 2 is an SEM image of CrVN 2 of the material prepared in example 1;
FIG. 3 is a graph of contact angle measurements of Pt/CrVN 2 material prepared in example 1;
FIG. 4 is a graph comparing gas-sensitive gradient tests of Pt/CrVN 2 sensor and Pt/C sensor.
Detailed Description
In the following description, specific details of the invention are set forth in order to provide a thorough understanding of the invention. The terminology used in the description of the invention herein is for the purpose of describing the advantages and features of the invention only and is not intended to be limiting of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The medicines or reagents used in the present invention are used according to the product instructions or by the conventional methods of use in the art unless specifically stated. The technical scheme of the invention is further described according to the attached drawings and the specific embodiments.
Example 1 (1), 2 mmol chromium chloride hexahydrate, 2 mmol vanadium chloride and 4mmol urea were placed in a 100mL beaker, followed by 50 mL deionized water into the beaker; placing the beaker into an ultrasonic instrument, and performing ultrasonic treatment for 30min to obtain a mixed solution;
(2) Transferring the mixed solution obtained in the step (1) into a polytetrafluoroethylene lining of 100 mL, loading the mixed solution into a stainless steel high-pressure reaction kettle, reacting 3h at 140 ℃ in an oven, and centrifugally collecting reactants after naturally cooling to room temperature, wherein the centrifugal collecting conditions are as follows: 10000 r/min, time: 5 min; washing the collected sample with deionized water for 3 times, and centrifugally collecting each time; washing the sample with absolute ethanol for 3 times, and centrifugally collecting each time; placing the collected sample into a vacuum drying oven, and drying at 60 ℃ for 8-12 h to obtain a tan powdery solid, namely CrVN 2 precursor;
(3) Taking the CrVN 2 precursor obtained in the step (2) of 200 mg, shaking to uniformly disperse the precursor in a porcelain boat, then placing the porcelain boat in a tube furnace, heating to 800 ℃ at 5 ℃/min under ammonia atmosphere to maintain 8 h, naturally cooling to room temperature after the procedure is finished, then introducing argon gas 1h to ensure that NH 3 is completely removed, and finally obtaining a black product, namely CrVN 2 material;
(4) Adding 50 mg of the H 2PtCl6 aqueous solution with the mass concentration of 100 mg/L and CrVN 2 and 340 mu L obtained in the step (3) into 50mL of ethylene glycol, wherein the mass ratio of CrVN 2 to Pt is 4:1, ultrasonic treatment is carried out for 30 to min until the mixture is uniformly mixed, then the mixed solution is transferred into a polytetrafluoroethylene lining, transferred into a stainless steel high-pressure reaction kettle, placed in an oven for heating at 140 ℃ for 3 h, reaction liquid is obtained, after the reaction liquid is naturally cooled to room temperature, reactants are centrifugally collected, and the centrifugal collection condition is the rotating speed: 10000 r/min, time: 5min, washing with deionized water for 3 times, washing with absolute ethyl alcohol for 3 times, centrifugally collecting each time, placing the collected sample into a vacuum drying oven, and drying at 60 ℃ for 8-12 h to obtain black powdery solid, namely the total product Pt/CrVN 2 material.
FIG. 1 is an XRD pattern for CrVN 2 and Pt/CrVN 2 materials prepared in example 1, showing successful synthesis of both CrVN 2 and Pt/CrVN 2 materials.
Fig. 2 is an SEM image of CrVN 2 material prepared in example 1, showing that the material exhibited a nanoparticle bulk state.
Example 2 (1), 1 mmol chromium chloride hexahydrate, 2 mmol vanadium chloride and 2 mmol urea were placed in a 100mL beaker, followed by 25 mL deionized water into the beaker; placing the beaker into an ultrasonic instrument, and performing ultrasonic treatment on the beaker for 40 min to obtain a mixed solution;
(2) Transferring the mixed solution obtained in the step (1) into a polytetrafluoroethylene lining of 100mL, loading the mixed solution into a stainless steel high-pressure reaction kettle, reacting at 160 ℃ in an oven for 6 h, and centrifugally collecting reactants after naturally cooling to room temperature, wherein the centrifugal collecting conditions are as follows: 8000 r/min, time: 10 min; washing the collected sample with deionized water for 3 times, and centrifugally collecting each time; washing the sample with absolute ethanol for 3 times, and centrifugally collecting each time; placing the collected sample into a vacuum drying oven, and drying at 40 ℃ for 8-12 h to obtain a tan powdery solid, namely CrVN 2 precursor;
(3) Taking the CrVN 2 precursor obtained in the step (2) of 200 mg, shaking to enable the precursor to be dispersed uniformly, then placing the ceramic boat into a tube furnace, heating to 700 ℃ at 3 ℃/min under ammonia atmosphere to maintain 6 h, naturally cooling to room temperature after the procedure is finished, then introducing argon gas 1h to ensure that NH 3 is completely removed, and finally obtaining a black product, namely CrVN 2 material;
(4) Adding 50 mg of the H 2PtCl6 aqueous solution with the mass concentration of 100mg/L and obtained in the step (3) and 340 mu L into 100mL ethylene glycol, carrying out ultrasonic treatment for 50 min until the aqueous solution is uniformly mixed, transferring the mixed solution into a polytetrafluoroethylene lining, transferring into a stainless steel high-pressure reaction kettle, placing into an oven for heating for 4H at 140 ℃ to obtain a reaction solution, centrifuging and collecting reactants after naturally cooling to room temperature, wherein the centrifuging and collecting conditions are as follows: 8000 r/min, time: 5min, washing with deionized water for 3 times, washing with absolute ethyl alcohol for 3 times, centrifugally collecting each time, placing the collected sample into a vacuum drying oven, and drying at 40 ℃ for 8-12 h to obtain black powdery solid, namely the total product Pt/CrVN 2 material.
Example 3 (1), 2 mmol chromium chloride hexahydrate, 1 mmol vanadium chloride and 3 mmol urea were placed in a 100mL beaker, and then 35 mL deionized water was added to the beaker; placing the beaker into an ultrasonic instrument, and performing ultrasonic treatment on the beaker for 60 min to obtain a mixed solution;
(2) Transferring the mixed solution obtained in the step (1) into a polytetrafluoroethylene lining of 100mL, loading the mixed solution into a stainless steel high-pressure reaction kettle, reacting 4h at 180 ℃ in an oven, and centrifugally collecting reactants after naturally cooling to room temperature, wherein the centrifugal collecting conditions are as follows: 9000 r/min, time: 7 min; washing the collected sample with deionized water for 3 times, and centrifugally collecting each time; washing the sample with absolute ethanol for 3 times, and centrifugally collecting each time; placing the collected sample into a vacuum drying oven, and drying at 50 ℃ for 8-12 h to obtain a tan powdery solid, namely CrVN 2 precursor;
(3) Taking the CrVN 2 precursor obtained in the step (2) of 200 mg, shaking to enable the precursor to be dispersed uniformly, then placing the ceramic boat into a tube furnace, heating to 600 ℃ at 4 ℃/min under ammonia atmosphere, maintaining the temperature at 8h, naturally cooling to room temperature after the procedure is finished, then introducing argon at 1.5 h to ensure that NH 3 is completely removed, and finally obtaining a black product, namely CrVN 2 material;
(4) Adding 100 mg H 2PtCl6 aqueous solution with the mass concentration of 100 mg/L obtained in the step (3) into 50mL glycol, carrying out ultrasonic treatment for 60: min until the aqueous solution is uniformly mixed, transferring the mixed solution into a polytetrafluoroethylene lining, transferring into a stainless steel high-pressure reaction kettle, placing into an oven, heating for 3H at 150 ℃ to obtain a reaction solution, centrifuging and collecting reactants after naturally cooling to room temperature, wherein the centrifuging and collecting conditions are as follows: 10000 r/min, time: 5min, washing with deionized water for 3 times, centrifugally collecting each time, washing the sample with absolute ethyl alcohol for 3 times, centrifugally collecting each time, placing the collected sample into a vacuum drying oven, and drying at 60 ℃ for 8-12 h to obtain black powdery solid, namely the total product Pt/CrVN 2 material.
Comparative example 1
(1) Adding 50mg carbon black and 340 mu L of H 2PtCl6 solution with the mass concentration of 100 mg/L into 50 mL glycol, carrying out ultrasonic treatment for 30min until the mixture is uniformly mixed, transferring the mixed solution into a polytetrafluoroethylene lining, transferring into a stainless steel high-pressure reaction kettle, placing the stainless steel high-pressure reaction kettle into an oven, heating for 3H at 140 ℃, and after the mixture is naturally cooled to room temperature, centrifugally collecting reactants, wherein the centrifugal collection condition is that the rotating speed is as follows: 10000 r/min, time: 5 min, washing with deionized water for 3 times, washing with absolute ethyl alcohol for 3 times, collecting the sample centrifugally, placing the collected sample into a vacuum drying oven, and drying at 60 ℃ for 8-12 h to obtain the Pt/C material.
Example 41 Performance test of Pt/CrVN 2 gas sensitive materials
The contact angle test of Pt/CrVN 2 was performed and the moisture resistance of the material was tested by a video optical contact angle meter. Fig. 3 is a graph of a contact angle test of the Pt/CrVN 2 material prepared in example 1, and the result shows that the contact angle of the material with water drops is 146.8 degrees, and the material has good moisture resistance.
2. Preparation and performance test of gas sensor
(1) Preparation of Pt/CrVN 2 gas sensor:
5mg of the Pt/CrVN 2 material prepared in example 1 was dissolved in 460. Mu.L of isopropanol solution and 40. Mu.L of Nafion solution (5 wt%) and thoroughly sonicated to obtain a catalyst ink. The obtained Pt/CrVN 2 catalyst ink was uniformly dropped on two pieces of 1.5 x 1.5 cm carbon paper, after being sufficiently dried, 20 μl of 5 wt% Nafion solution was uniformly dropped on the catalyst layer, and then dried again in an oven. The treated carbon paper was cut into a round shape with a diameter of 1 cm a. Finally, two layers of carbon paper and one layer of Nafion membrane were hot pressed at 90 ℃ and 1.5 MPa to obtain a Membrane Electrode Assembly (MEA). Then bonding the MEA and the stainless steel electrode cap and the water storage tank together to obtain the Pt/CrVN 2 sensor to be operated
(2) Preparation of Pt/C gas sensor:
The Pt/C prepared in comparative example 1, 5 mg, was dissolved in 460. Mu.L of isopropanol solution and 40. Mu.L of Nafion solution (5 wt%) and sufficiently sonicated to obtain a catalyst ink. The obtained Pt/C catalyst ink was uniformly dropped on two pieces of 1.5 x 1.5 cm carbon paper, and after sufficient drying, 20. Mu.L of 5 wt% Nafion solution was uniformly dropped on the catalyst layer, and then dried again in an oven. The treated carbon paper was cut into a round shape with a diameter of 1 cm a. Finally, two layers of carbon paper and one layer of Nafion membrane were hot pressed at 90 ℃ and 1.5 MPa to obtain a Membrane Electrode Assembly (MEA). Then bonding the MEA and the stainless steel electrode cap and the water storage tank together to obtain the Pt/C sensor to be operated
(3) Performance testing of gas sensors
The Pt/CrVN 2 sensor and the Pt/C sensor are respectively connected with an electrochemical workstation, hydrogen sulfide gas of 1-100 ppm is sequentially introduced, and a comparison chart of gas-sensitive gradient tests of the Pt/CrVN 2 sensor and the Pt/C sensor shows that the Pt/CrVN 2 sensor has excellent performance on the hydrogen sulfide gas, the response current is 15.6 mu A at the concentration of 50 ppm, and the response current of the Pt/C sensor is only 7.5 mu A.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the essence of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The preparation method of the Pt/CrVN 2 gas-sensitive electrode material is characterized by comprising the following steps of:
(1) Taking a chromium source, a vanadium source and urea, adding deionized water, and performing ultrasonic treatment to obtain a mixed solution;
(2) Heating the mixed solution obtained in the step (1), centrifuging to collect reactants, and drying in vacuum to obtain CrVN 2 precursor;
(3) Calcining the CrVN 2 precursor obtained in the step (2) to obtain CrVN 2 material;
(4) Mixing CrVN 2 material obtained in the step (3), glycol and H 2PtCl6 water solution, performing ultrasonic treatment, and performing heating reaction to obtain a reaction solution;
(5) And (3) centrifuging the reaction liquid obtained in the step (4), and vacuum drying to obtain the Pt/CrVN 2 gas-sensitive electrode material.
2. The method of claim 1, wherein in step (1), the chromium source is chromium chloride hexahydrate and the vanadium source is vanadium chloride;
the mole volume ratio of the chromium source, the vanadium source, the urea and the deionized water is (1-2) mmol: (1-2) mmol: (2-4) mmol: (25-50) mL;
The ultrasonic treatment time is 30-60 min.
3. The method according to claim 1, wherein in the step (2), the heating reaction is carried out at a temperature of 140 to 180 ℃ for a time of 3 to 6 h;
Cooling to room temperature after the heating reaction;
the rotational speed of the centrifugation is 8000-10000 r/min, and the time is 5-10 min;
The vacuum drying temperature is 40-60 ℃ and the time is 8-12 h.
4. The method according to claim 1, wherein in the step (3), the calcination is performed under an ammonia atmosphere at 600-800 ℃ for 6-8 h ℃ and at a heating rate of 3-5 ℃/min;
And cooling to room temperature after calcination, and introducing argon gas 1-1.5 h.
5. The method according to claim 1, wherein in the step (4), the mass concentration of the aqueous solution of H 2PtCl6 is 100 mg/L;
The mass volume ratio of the CrVN 2 material to the glycol to the H 2PtCl6 aqueous solution is (5-10) mg: (5-10) mL: (34-68) μl.
6. The method of claim 1, wherein in step (4), the time of the ultrasonic treatment is 30 to 60 min;
The temperature of the heating reaction is 140-150 ℃ and the time is 3-4 h.
7. The method according to claim 1, wherein in the step (5), the rotational speed of the centrifugation is 8000-10000 r/min for 5-min;
The vacuum drying temperature is 40-60 ℃ and the time is 8-12 h.
8. A Pt/CrVN 2 gas sensitive electrode material prepared by the method of any one of claims 1 to 7.
9. Use of the Pt/CrVN 2 gas sensitive electrode material prepared by the method of any one of claims 1-7 and/or the Pt/CrVN 2 gas sensitive electrode material of claim 8, for the preparation of a gas sensor.
10. The use of claim 9, wherein the gas sensor is for detecting H 2 S gas.
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