CN118563360A - Mesoporous Au-based alloy thin film catalyst and preparation method thereof - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims abstract description 61
- 239000010409 thin film Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000010408 film Substances 0.000 claims abstract description 38
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006056 electrooxidation reaction Methods 0.000 claims abstract description 15
- 238000001659 ion-beam spectroscopy Methods 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 8
- 150000003624 transition metals Chemical class 0.000 claims abstract description 7
- 229910052737 gold Inorganic materials 0.000 claims abstract description 6
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- 238000000034 method Methods 0.000 claims abstract 9
- 239000010931 gold Substances 0.000 claims description 86
- 238000004140 cleaning Methods 0.000 claims description 28
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- 238000001035 drying Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
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- 229910000636 Ce alloy Inorganic materials 0.000 abstract description 17
- 238000005530 etching Methods 0.000 abstract description 12
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- 229910000905 alloy phase Inorganic materials 0.000 abstract 1
- 238000007737 ion beam deposition Methods 0.000 abstract 1
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- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
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Abstract
The invention discloses a mesoporous Au-based alloy thin film catalyst and a preparation method thereof, and belongs to the technical field of electrocatalysis. According to the invention, au is used as a main phase catalyst element, a transition metal element is used as an alloy phase, a rare earth element is used as a cocatalyst, an Au-based alloy film is prepared on a carbonaceous carrier by adopting an ion beam deposition method, and an HClO 4 and NaF mixed solution system is used for carrying out electrochemical corrosion on the Au-based alloy film, so that the mesoporous Au-based alloy film catalyst is obtained. According to the invention, the active center of CO 2 ERR is increased through the mutual synergistic effect of Au, ti and Ce in the Au-Ti-Ce alloy catalyst, and the CO 2 ERR performance is improved. Meanwhile, the Au-Me-Re alloy film obtained by ion beam sputtering is selectively corroded through a mixed solution system of HClO 4 and NaF, transition metal is removed by etching, the content of Au is improved, a mesoporous material is constructed, and the CO 2 ERR performance and the electrocatalytic activity of the material are obviously improved.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis, and particularly relates to a mesoporous Au-based alloy thin film catalyst and a preparation method thereof.
Background
Carbon dioxide is the main gas causing the greenhouse effect, solving carbon dioxide emissions can start from two aspects, first: optimizing energy mode, and replacing traditional energy with new energy. Although new energy is rapidly developed at present, the complete replacement of traditional energy by new energy is not possible. Second,: photocatalysis and electrocatalysis may be used to convert CO 2 to other more valuable chemicals. The photocatalysis synthesis method is complex, the solar spectrum utilization rate is low, the electrocatalytic synthesis method is relatively simple, and the reaction condition is mild. The electrocatalytic core is a membrane catalyst, and an Au-based material with low overpotential and good product selectivity is generally selected.
In the design and preparation of mesoporous Au-based alloy film, chinese patent application CN105107499a uses HClO 4 to perform electrochemical dealloying on Au-based catalyst to obtain nano-porous catalyst with small pore size and large specific surface area, but dealloying time is long and selective etching of alloy element is not possible. The Chinese patent CN105063399A uses NaOH solution to conduct dealloying to obtain porous nano metal, which has large specific surface area and good conductivity, but the pore size is 30-170nm and does not belong to mesoporous structure. Therefore, it is important to explore a preparation method of the mesoporous Au-based alloy film catalyst, and solve the problems of long corrosion time, noble metal loss and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a mesoporous Au-based alloy thin film catalyst and a preparation method thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a preparation method of a mesoporous Au-based alloy thin film catalyst comprises the following steps:
(1) Pretreating a carbon carrier to obtain a pretreated carbon carrier;
(2) Placing the pretreated carbonaceous carrier on an ion beam sputtering sample stage, then mounting a gold target, a transition metal target and a rare earth element target on the target stage, cleaning the carbonaceous carrier, and then performing ion beam sputtering to obtain an Au-based alloy film;
(3) And (3) putting the Au-based alloy film into a mixed solution system of HClO 4 and NaF for electrochemical corrosion to obtain the mesoporous Au-based alloy film catalyst.
As a preferred embodiment of the present invention, the mass concentration ratio of HClO 4 to NaF in the mixed solution of HClO 4 and NaF is 0.01-0.3:0.0048.
As a preferred embodiment of the present invention, the carbonaceous carrier is one of a graphite fiber cloth, a carbon paper or a graphite sheet.
As a preferred embodiment of the present invention, the pretreatment specifically includes: and (3) placing the carbon carrier into a 0.5M H 2SO4 solution for ultrasonic cleaning, then placing into acetone for ultrasonic cleaning, then placing into water for ultrasonic cleaning, finally placing into absolute ethyl alcohol for soaking, taking out the carbon carrier and drying.
As a preferred embodiment of the present invention, in the step (2), the cleaning parameters include: the heating temperature is 190-210 ℃, the vacuum is pumped to 5.0X10 -4～8.0×10-4 Pa, the cleaning is carried out when the vacuum degree is 1.2X10 -2～1.4×10-2 Pa, the cleaning time is 5-15 min, and the cleaning gas is N 2 and Ar.
As a preferred embodiment of the present invention, in the step (2), the parameters of the ion beam sputtering include: the gas is N 2 and Ar, the flow rate of N 2 is 5.0-6.0 sccm, and the flow rate of Ar is 9.0-10.0 sccm; the screen voltage is 2KV, the beam current is 70mA, the cathode current is 15A, the anode voltage is 40V, the time is 10-20 min, and the vacuum degree is 1.2X10 -2～1.4×10-2 Pa.
As a preferred embodiment of the present invention, the transition metal target is a Ti target; the rare earth element target is a Ce target.
As a preferred embodiment of the invention, the electrochemical corrosion temperature is 18-30 ℃ and the corrosion time is 150-250S;
the invention also claims a mesoporous Au-based alloy film prepared by the preparation method of the mesoporous Au-based alloy film catalyst.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, the active center of CO 2 ERR is increased through the mutual synergistic effect of Au, ti and Ce in the Au-Me-Re alloy catalyst, and the CO 2 ERR performance is improved. The transition metal Ti can interact with Au, so that the dosage of Au is reduced, and the catalytic activity of Au is improved; the addition of the rare earth element Ce can increase oxygen vacancies and provide more transfer channels for free electrons, and Ce is easily oxidized into CeO 2,CeO2 which can form an active interface by interaction with Au. Meanwhile, ti can change the oxygen vacancy forming energy of CeO 2 and increase the free electron concentration around Au, so that the CO 2 ERR performance and the electrocatalytic activity are remarkably enhanced.
(2) According to the invention, the Au-Me-Re alloy film obtained by ion beam sputtering is selectively etched through the HClO 4 and NaF system, the transition metal Ti is removed by etching, the Au content is improved, the mesoporous material is constructed, and the CO 2 ERR performance and the electrocatalytic activity of the material are obviously improved.
(3) The invention adopts ion beam sputtering technology, can enhance the bonding strength and conductivity of the Au-based alloy catalyst film layer and the carbonaceous carrier, thereby improving the selective corrosion of the Au-Me-Re alloy film by the acid and auxiliary agent system and the electrocatalytic activity of the Au-based alloy film catalyst.
Drawings
FIG. 1 is an LSV graph of Au-based alloy thin film catalysts prepared in comparative examples 1 to 4.
FIG. 2 is an LSV diagram of the mesoporous Au-based alloy thin film catalysts prepared in examples 1 to 3.
FIG. 3 is a STEM chart of the Au-based alloy thin film catalyst prepared in comparative example 1.
FIG. 4 is a STEM chart of the mesoporous Au-based alloy thin film catalyst prepared in example 1.
Fig. 5 is a graph showing pore size distribution curves of the mesoporous Au-based alloy thin film catalyst prepared in example 1 and the Au-Ti-Ce alloy thin film before etching, the graph showing pore size distribution curves of the Au-Ti-Ce alloy thin film before etching prepared in example 1, and the graph showing pore size distribution curves of the mesoporous Au-based alloy thin film catalyst prepared in example 1.
Fig. 6 is a graph showing pore size distribution curves of the mesoporous Au-based alloy thin film catalyst prepared in example 2 and the Au-Ti-Ce alloy thin film before etching, the upper graph shows pore size distribution curves of the Au-Ti-Ce alloy thin film before etching prepared in example 2, and the lower graph shows pore size distribution curves of the mesoporous Au-based alloy thin film catalyst prepared in example 2.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
A preparation method of a mesoporous Au-based alloy thin film catalyst comprises the following steps:
(1) Placing the rectangular graphite fiber cloth with the length of 16 multiplied by 15cm into H 2SO4 with the length of 0.5M, ultrasonically cleaning for 15min, placing the graphite fiber cloth with the length of H 2SO4, ultrasonically cleaning for 15min, placing into deionized water, ultrasonically cleaning for 15min, finally placing into absolute ethyl alcohol, soaking for 2min, dehydrating, taking out the graphite fiber cloth, and drying.
(2) Placing the pretreated graphite fiber cloth on an ion beam sputtering sample table, then mounting an Au target, a Ti target and a Ce target on the target table, heating the sample to 200 ℃, vacuumizing to 8.0X10 -4 Pa, cleaning when the vacuum degree is 1.4X10 -2 Pa, cleaning for 10min with N 2 and Ar as cleaning gas, then introducing 9sccmAr and 6sccmN 2 flow, wherein the screen pressure is 2kV, the beam current is 70mA, the cathode current is 15A, the anode voltage is 40V, the vacuum degree is 1.4X10 -2 Pa, generating the ion beam sputtering Au target, the Ti target and the Ce target, sputtering for 15min, and annealing and cooling to obtain the Au-Ti-Ce alloy film.
(3) Cutting the obtained Au-Ti-Ce alloy film into a sample with the length of 2 multiplied by 2cm, and then placing the Au-based alloy film into a 0.2M mixed solution system of HClO 4 and 0.0048MNaF for electrochemical corrosion, wherein the temperature of the electrochemical corrosion is 20 ℃, the time is 200S, and the potential is 1.2V. Obtaining the mesoporous Au-based alloy film catalyst.
Example 2
A preparation method of a mesoporous Au-based alloy thin film catalyst comprises the following steps:
(1) Placing the rectangular graphite fiber cloth with the length of 16 multiplied by 15cm into H 2SO4 with the length of 0.5M, ultrasonically cleaning for 15min, placing the graphite fiber cloth with the length of H 2SO4, ultrasonically cleaning for 15min, placing into deionized water, ultrasonically cleaning for 15min, finally placing into absolute ethyl alcohol, soaking for 2min, dehydrating, taking out the graphite fiber cloth, and drying.
(2) Placing the pretreated graphite fiber cloth on an ion beam sputtering sample table, then mounting an Au target, a Ti target and a Ce target on the target table, heating the sample to 190 ℃, vacuumizing to 5.0x10 -4 Pa, cleaning when the vacuum degree is 1.2x10 -2 Pa, cleaning for 5min with N 2 and Ar as cleaning gas, then introducing 10sccmAr and 5sccmN 2 flow, wherein the screen pressure is 2kV, the beam current is 70mA, the cathode current is 15A, the anode voltage is 40V, the vacuum degree is 1.2x10 -2 Pa, generating the ion beam sputtering Au target, the Ti target and the Ce target, sputtering for 20min, and annealing and cooling to obtain the Au-Ti-Ce alloy film.
(3) Cutting the obtained Au-Ti-Ce alloy film into a sample with the length of 2 multiplied by 2cm, and then placing the Au-based alloy film into a 0.3M mixed solution system of HClO 4 and 0.0048MNaF for electrochemical corrosion, wherein the temperature of the electrochemical corrosion is 20 ℃, the time is 250S, and the potential is 0.8V. Obtaining the mesoporous Au-based alloy film catalyst.
Example 3
A preparation method of a mesoporous Au-based alloy film catalyst comprises the following steps:
(1) Placing the rectangular graphite fiber cloth with the length of 16 multiplied by 15cm into H 2SO4 with the length of 0.5M, ultrasonically cleaning for 15min, placing the graphite fiber cloth with the length of H 2SO4, ultrasonically cleaning for 15min, placing into deionized water, ultrasonically cleaning for 15min, finally placing into absolute ethyl alcohol, soaking for 2min, dehydrating, taking out the graphite fiber cloth, and drying.
(2) Placing the pretreated graphite fiber cloth on an ion beam sputtering sample table, then mounting an Au target, a Ti target and a Ce target on the target table, heating the sample to 210 ℃, vacuumizing to 7.0X10 -4 Pa, cleaning when the vacuum degree is 1.3X10 -2 Pa, cleaning for 15min with N 2 and Ar as cleaning gas, introducing 9sccmAr and 5.5sccmN 2 flow, setting the screen pressure at 2kV, setting the beam current at 70mA, setting the cathode current at 15A, setting the anode voltage at 40V, setting the vacuum degree at 1.0X10 -2 Pa, generating the ion beam sputtering Au target, ti target and Ce target, sputtering for 5min, and annealing and cooling to obtain the Au-Ti-Ce alloy film.
(3) Cutting the obtained Au-Ti-Ce alloy film into a sample with the length of 2 multiplied by 2cm, and then placing the Au-based alloy film into a 0.1M mixed solution system of HClO 4 and 0.0048MNaF for electrochemical corrosion, wherein the temperature of the electrochemical corrosion is 25 ℃, the time is 200S, and the potential is 1.0V. Obtaining the mesoporous Au-based alloy film catalyst.
Comparative example 1
The only difference between the preparation method of the Au-based alloy thin film catalyst of the comparative example and the preparation method of the Au-based alloy thin film catalyst of the example 1 is that: in the step (3), the Au-based alloy film is put into 0.01M HCl solution for electrochemical corrosion.
Comparative example 2
The only difference between the preparation method of the Au-based alloy thin film catalyst of the comparative example and the preparation method of the Au-based alloy thin film catalyst of the example 1 is that: in the step (2), the targets are Au targets and Ti targets, and the Au-Ti alloy film is obtained.
Comparative example 3
The only difference between the preparation method of the Au-based alloy thin film catalyst of the comparative example and the preparation method of the Au-based alloy thin film catalyst of the example 1 is that: in the step (2), the targets are Au targets and Ce targets, and the Au-Ce alloy film is obtained.
Comparative example 4
The only difference between the preparation method of the Au-based alloy thin film catalyst of the comparative example and the preparation method of the Au-based alloy thin film catalyst of the example 1 is that: in the step (2), the target material is an Au target, and a pure Au film is obtained.
Comparative example 5
The only difference between the preparation method of the Au-based alloy thin film catalyst of the comparative example and the preparation method of the Au-based alloy thin film catalyst of the example 1 is that: in the step (3), the Au-based alloy film is put into a 0.2M HClO 4 solution for electrochemical corrosion.
Comparative example 6
The only difference between the preparation method of the Au-based alloy thin film catalyst of the comparative example and the preparation method of the Au-based alloy thin film catalyst of the example 1 is that: in the step (3), the Au-based alloy film is put into a NaF solution of 0.0048M for electrochemical corrosion.
Effect example
Test sample: examples 1 to 3 and comparative examples 1 to 6.
The testing method comprises the following steps: (1) Characterizing the surface morphology of the test sample by scanning a special electron microscope (STEM); the pore size of the test samples was characterized by BET test and the ICP test element content is shown in table 1.
(2) The activity of Au-based thin film catalysts was characterized using Linear Sweep Voltammetry (LSV) using a three electrode system of an electrochemical workstation in combination. The LSV test scanning interval is-0.40-0.20V (relative to a saturated calomel electrode), the scanning rate is 50mv/s, i 0 and eta are calculated through a formula (1), in the hydrogenation performance research of the Au-based catalyst, i 0 and eta of an LSV curve are often adopted to represent the hydrogenation activity, and the result is shown in Table 2.
η=a+blog|i0| （1）
Where η is the overpotential, i 0 is the current density, a is a constant, and b is the Tafel slope.
TABLE 1
TABLE 2
As can be seen from fig. 3 to 4 and 5 to 6, the Au-Ti-Ce alloy thin films prepared in comparative examples 1, 4 and examples all formed holes and mesoporous materials after electrochemical corrosion. Examples 1 to 3 and comparative examples 1 to 5 were subjected to electrochemical etching to form mesoporous materials, and comparative example 6 was not formed with mesoporous materials, which were denser materials having similar morphology to the au—ti-Ce alloy films before the etching of examples 1 to 3. According to tables 1 and 2, according to the invention, by compounding HClO 4 and NaF, ti can be selectively etched, the content of Au is increased, and the catalytic performance of the material is further improved. The HClO 4 +NaF system selectively etches Ti in the Au-Ti-Ce alloy, so that the surface area of the porous material is increased, more attachment points are provided for CO 2 adsorption, the relative content of noble metals is improved, the surface property of the porous material is changed, and the catalytic performance is improved. Comparative examples 1 and 5 used HCl solution and HClO 4 solution to electrochemically etch Au-Ti-Ce catalyst, respectively, while Au, ti and Ce were etched, and Au was etched in a large amount, active sites were lost in a large amount, and the performance of the catalyst was greatly reduced. Comparative example 3 Au-Ce alloy catalyst was etched using HClO 4 and NaF, in which Au and Ce were simultaneously etched in a large amount, resulting in degradation of the catalyst performance. Comparative example 6 the performance of the Au-Ti-Ce alloy thin film catalyst using NaF was not as good as that of comparative example 4. Compared with example 1, comparative example 2 uses HClO 4 + NaF system to etch au—ti alloy, and the variation of Au etching is similar to example 1 due to lack of Ce alloying, but the variation of Ti etching is reduced, so that the selective etching of Ti is reduced, and the performance data is also significantly reduced.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. The preparation method of the mesoporous Au-based alloy thin film catalyst is characterized by comprising the following steps of:
(1) Pretreating a carbon carrier to obtain a pretreated carbon carrier;
(2) Placing the pretreated carbonaceous carrier on an ion beam sputtering sample stage, then mounting a gold target, a transition metal target and a rare earth element target on the target stage, cleaning the carbonaceous carrier, and then performing ion beam sputtering to obtain an Au-based alloy film;
(3) And (3) putting the Au-based alloy film into a mixed solution of HClO 4 and NaF for electrochemical corrosion to obtain the mesoporous Au-based alloy film catalyst.
2. The method for preparing a mesoporous Au based alloy thin film catalyst according to claim 1, wherein the mass concentration ratio of the substances HClO 4 and NaF in the mixed solution of HClO 4 and NaF is 0.01-0.3:0.0048.
3. The method for preparing a mesoporous Au based alloy thin film catalyst according to claim 1, wherein the carbonaceous carrier is one of graphite fiber cloth, carbon paper or graphite sheet.
4. The method for preparing a mesoporous Au-based alloy thin film catalyst according to claim 1, wherein the pretreatment specifically comprises: and (3) placing the carbon carrier into a 0.5M H 2SO4 solution for ultrasonic cleaning, then placing into acetone for ultrasonic cleaning, then placing into water for ultrasonic cleaning, finally placing into absolute ethyl alcohol for soaking, taking out the carbon carrier and drying.
5. The method for preparing a mesoporous Au based alloy thin film catalyst according to claim 1, wherein in the step (2), the cleaning parameters include: the heating temperature is 190-210 ℃, the vacuum is pumped to 5.0X10 -4～8.0×10-4 Pa, the cleaning is carried out when the vacuum degree is 1.2X10 -2～1.4×10-2 Pa, the cleaning time is 5-15 min, and the cleaning gas is N 2 and Ar.
6. The method for preparing a mesoporous Au based alloy thin film catalyst according to claim 5, wherein in the step (2), parameters of ion beam sputtering include: the gas is N 2 and Ar, the flow rate of N 2 is 5.0-6.0 sccm, and the flow rate of Ar is 9.0-10.0 sccm; the screen voltage is 2KV, the beam current is 70mA, the cathode current is 15A, the anode voltage is 40V, the time is 10-20 min, and the vacuum degree is 1.2X10 -2～1.4×10-2 Pa.
7. The method for preparing a mesoporous Au based alloy thin film catalyst according to claim 1, wherein the transition metal target is a Ti target and the rare earth element target is a Ce target.
8. The method for preparing a mesoporous Au-based alloy thin film catalyst according to claim 1, wherein the electrochemical corrosion temperature is 18-30 ℃, the corrosion time is 150-250S, and the potential is 0.8-1.2V.
9. A mesoporous Au-based alloy thin film prepared by the method for preparing a mesoporous Au-based alloy thin film catalyst according to any one of claims 1 to 8.
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