CN113281396A - Catalyst performance characterization method based on improved SECM probe - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims abstract description 67
- 239000000523 sample Substances 0.000 title claims abstract description 57
- 238000001115 scanning electrochemical microscopy Methods 0.000 title claims abstract description 37
- 238000012512 characterization method Methods 0.000 title claims abstract description 12
- 239000000376 reactant Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 23
- 238000012360 testing method Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000002184 metal Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000011148 porous material Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 17
- 238000005530 etching Methods 0.000 claims description 8
- 230000003287 optical effect Effects 0.000 claims description 7
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 6
- 230000007797 corrosion Effects 0.000 claims description 6
- 238000004502 linear sweep voltammetry Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 13
- 238000006555 catalytic reaction Methods 0.000 abstract description 13
- 238000011049 filling Methods 0.000 abstract description 8
- 230000007246 mechanism Effects 0.000 abstract description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 10
- 239000010931 gold Substances 0.000 description 9
- 229910001323 Li2O2 Inorganic materials 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 239000011949 solid catalyst Substances 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 5
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 5
- 238000000227 grinding Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000004913 activation Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 description 2
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(IV) oxide Inorganic materials O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 230000005641 tunneling Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 238000002847 impedance measurement Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004621 scanning probe microscopy Methods 0.000 description 1
- 238000004574 scanning tunneling microscopy Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
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Abstract
The invention provides a catalyst performance characterization method based on an improved SECM probe, which comprises the following steps: and filling the catalyst powder to be detected into the improved SECM probe, and performing electrochemical performance characterization on the catalyst by using a scanning electrochemical microscope. According to the method for characterizing the catalyst performance, the SECM provided with the improved probe is utilized, and the electrochemical performance characterization means is combined to characterize the catalytic performance of the catalyst, so that the metal wire in the probe is directly contacted with the catalyst, the catalytic reaction performance between the catalyst and a reactant is tested, the accuracy of the catalytic reaction test can be effectively improved, the catalytic mechanism is better revealed, and guidance is provided for optimizing the catalytic conditions of the catalyst. In addition, the contact between the catalyst and the target reactant can be better realized by adjusting the pressure of the SECM on the target reactant, and the accuracy of the catalytic reaction test is further improved.
Description
Technical Field
The invention belongs to the technical field of solid-solid interface property and catalytic reaction characterization, and particularly relates to a catalyst performance characterization method based on an improved SECM probe.
Background
It is well known that any chemical reaction occurs by overcoming a certain energy barrier to reach an active state and thus a corresponding chemical reaction occurs. The energy required to change from the ground state to the activated state is the activation energy Ea, and the activation energy required for some reactions is too high to allow the target reaction to occur. For this reason, the advent of catalysts has addressed this problem well, as rational use of catalysts can effectively lower the activation energy of the target reaction, thereby accelerating the reaction.
In view of the fact that the performance of most of the current solid catalysts is generally determined only by the advantages and disadvantages of the performance, the catalytic mechanism is summarized simply by the characterization of the whole catalyst, and the like, and the optimization means of the factors such as the contact property of the catalyst is also deficient. On the basis, various electrochemical characterization means are provided for detecting and characterizing the catalytic performance of the catalyst for catalyzing the solid reaction to be detected.
Because most of common catalysts are solid, the detection of the catalytic performance of the catalyst in the prior art generally includes loading a certain catalyst on a corresponding carrier (generally adopting carbon paper), thereby catalyzing a target reactant. The introduction of the carrier can increase the impedance during reaction, reduce the reaction activity and influence the detection result to reduce the accuracy. In addition, the catalyst is loaded on a corresponding carrier, and generally a smearing mode is adopted for loading, so that uneven smearing is easily caused, interference in detection is increased, and the detection result is also influenced.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a catalyst performance characterization method based on an improved SECM probe, so as to more accurately reveal the catalytic reaction mechanism of a solid catalyst for catalyzing a solid reactant to be detected, thereby optimizing the catalyst performance and improving the efficiency of related chemical reactions.
A method for characterizing catalyst performance based on an improved SECM probe, comprising: and mounting the improved SECM probe filled with the catalyst powder to be detected on a scanning electrochemical microscope, pressing the probe on the solid reactant, and performing electrochemical performance characterization on the catalyst-catalyzed solid reactant.
Scanning electrochemical microscopy (SECM) is a scanning probe microscopy technique proposed and developed by the a.j.bard group in the 80 s. It was developed based on Ultramicroelectrodes (UME) and scanning tunneling microscopy. Based on the electrochemical reaction principle, the scanning tunneling microscope can be flexibly combined with other research methods and technologies for use, and the scanning skill of the scanning tunneling microscope can help measure information such as electrochemical reaction kinetics in a micro-area.
In the technical scheme, the metal electrode is directly contacted with the catalyst by utilizing the scanning function of the SECM, and the catalytic reaction of the catalyst is correspondingly detected by combining an electrochemical characterization means, so that the catalytic mechanism is better revealed, and guidance is provided for selecting the catalyst and the catalytic reaction condition.
Preferably, the catalyst is electrochemically characterized using one of impedance measurements (EIS), Linear Sweep Voltammetry (LSV).
Preferably, when the electrochemical performance of the catalyst is characterized by using a scanning electrochemical microscope, the corresponding wire clamp for electrochemical test is clamped on the corresponding electrode sheet.
Preferably, the modified SECM probe is a microelectrode with an aperture at the end for receiving the catalyst powder to be detected.
In the technical scheme, the microelectrode is structurally characterized in that a metal wire is embedded in glass and is integrally sintered with the glass, wherein the metal wire is a platinum wire or a gold wire.
More preferably, in the micro-electrode, the diameter of the metal wire is 5 to 100 μm.
Preferably, the particle size of the catalyst powder is 2 to 200 nm.
Preferably, the improved SECM probe is prepared by the following method:
and corroding the end part of the microelectrode, forming a pore for containing the powder to be detected in the microelectrode, and performing post-treatment to obtain the improved SECM probe.
The depth of the pores is determined according to the etching time, and the etching depth can be measured by an optical microscope, wherein the etching depth is preferably 1-20 mu m.
Preferably, when the microelectrode is corroded, hot aqua regia or concentrated hydrochloric acid is used as a corrosive liquid; when hot aqua regia is used, the corrosion temperature is 100 ℃.
Preferably, the microelectrodes are maintained in constant axial rotation during the etching of the microelectrodes. The technical scheme is adopted to ensure that the corroded end face of the metal wire is tidy so as to better clean the pores.
Preferably, after the etching of the end portion of the micro-electrode is completed, the following post-treatment is performed:
and ultrasonically cleaning the probe by using ethanol for 3-5 times, and drying to obtain the probe.
The ultrasonic cleaning by adopting ethanol aims to remove residual corrosive liquid, prevent the corrosive liquid from further corroding the metal wire to cause irregular end surfaces and increase the cleaning difficulty.
Specifically, the preparation method of the improved SECM probe comprises the following steps: immersing the end part of the microelectrode into a corrosive liquid, corroding under the condition of constant-speed axial rotation, ultrasonically cleaning for 3-5 times by using ethanol after the corrosion is finished, and drying to obtain the probe.
Preferably, the catalyst powder to be detected is loaded into the pores of the probe in an ink-milled manner. Because the pore space is very small, filling by adopting an ink grinding mode can realize that the catalyst powder is filled into the pore space, and the pressure applied to the probe in the filling process can ensure that the catalyst powder is firmly filled.
Preferably, when the catalyst powder is loaded into the pores, whether the pores are filled with the catalyst powder is observed with an optical microscope. And whether the pores are filled is observed by adopting an optical microscope so as to ensure that the catalyst is fully contacted with the reactant during the subsequent reaction with the reactant, and the accuracy of the detection result is further improved.
Preferably, the modified SECM probe is provided with a pressure sensor for monitoring and regulating the pressure with which the modified SECM probe is pressed against the solid reactant.
In the above technical solution, the pressure sensor may be selectively integrated on the modified SECM probe, so as to realize pressure adjustment of the modified SECM probe pressing on the solid reactant, and further realize adjustment of the contact pressure of the solid catalyst and the solid reactant. By using the pressure sensor, on one hand, whether the improved SECM probe (solid catalyst) is effectively contacted with a substrate (solid reactant) can be detected, so that the solid catalyst is ensured to be fully contacted with the solid reactant, and the accuracy of a detection result is improved; on the other hand, the magnitude of the specific contact force between the solid catalyst and the solid reactant can be known.
As a specific preference, a method for characterizing catalyst performance based on an improved SECM probe, comprising:
placing the catalyst powder to be detected on a flat glass plate, holding the improved SECM probe by hand, filling the catalyst powder to be detected into the pore of the probe in an ink grinding mode, and observing whether the pore is filled by using an optical microscope after filling; the modified SECM probe with the pores filled with the catalyst powder was mounted on the SECM and pressed against the solid reactant to bring the catalyst into full contact with the solid reactant (as determined by the pressure sensor), and the corresponding electrochemical test was performed with the electrode clamped by the wire clamp for electrochemical test.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for characterizing the catalyst performance, the SECM provided with the improved probe is utilized, and the electrochemical performance characterization means is combined to characterize the catalytic performance of the catalyst, so that the metal electrode in the probe is directly contacted with the catalyst, the catalytic reaction performance between the catalyst and a reactant is tested, the accuracy of the catalytic reaction test can be effectively improved, the catalytic mechanism is better revealed, and guidance is provided for optimizing the catalytic conditions of the catalyst.
In addition, the contact between the catalyst and the target reactant can be better realized by adjusting the pressure of the SECM on the target reactant, and the accuracy of the catalytic reaction test is further improved.
Drawings
FIG. 1 is a microscopic end view of the Pt probe prepared in example 1;
FIG. 2 is a diagram showing that the Pt probe prepared in example 1 is filled with MnO2Posterior end micrographs;
FIG. 3 shows the load MnO in example 12The structure schematic diagram of the Pt probe for detecting the catalytic performance;
FIG. 4 shows MnO supported on Pt probe and carbon paper in example 12Catalytic Li2O2Comparative graphs of EIS of the reactions;
FIG. 5 shows RuO loaded on Au probe in example 22Catalytic Li2O2LSV profile of reaction.
Detailed Description
Example 1
Soaking the end part of a Pt microelectrode with the diameter of 25 mu m in hot aqua regia at 100 ℃ for corrosion for 5min (keeping the Pt microelectrode rotating at a constant axial speed and the rotating speed of 10 r/min), then ultrasonically washing for 3 times by using ethanol, and drying to obtain the Pt probe with a pore with the corrosion depth of about 1 mu m at the end part. As shown in FIG. 1, which is a microscopic view of the tip of the Pt probe, it can be seen that the tip of the Pt microelectrode was successfully etched.
Filling MnO into the Pt probe by adopting an ink grinding mode2Powder (particle size 30 nm). The end micrographs after filling are shown in FIG. 2, which FIG. 2 shows the middle pore is black, demonstrating MnO2The powder filling was successful.
The Pt probe was mounted on SECM in Li2O2Impedance tests (EIS) were performed on any two different spots on the sheet, point a and point B, as experimental groups. A control group was also set: MnO of2MnO preparation after mixing powder (particle size 30nm, 0.022g), PTFE binder (10% PTFE, 0.048g) and ethanol (2ml)2Slurry of MnO2Uniformly coating the slurry on carbon paper, and standing; when the ethanol is completely volatilized (the thickness of the dry film is about 1 mu m), the carbon paper is coated with MnO2One side of which is covered with the reactant, and a 25 mu mPT planar electrode is respectively pressed against the carbon paper at A1、B1The test was performed at two different points.
The impedance tests of the experimental group and the control group are carried out in 0.5M LiTFSI TEGDME electrolyte, a platinum wire is used as a counter electrode, a silver wire is used as a reference electrode, and a Pt probe and a Pt planar electrode are respectively used as corresponding working electrodes. During testing, the wire clamps of the EIS are respectively clamped on the corresponding electrodes.
Load MnO2Pt probe and reactant Li2O2The schematic structure of the sheet contact test is shown in FIG. 3, in which 1 is a corroded microelectrode, 1' is a filled catalyst powder, and 2 is a pressure sensorAnd 3 is the target reactant Li2O2And (3) slicing.
The Pt probe and the Pt planar electrode are pressed on the reactant Li when the pressure sensor is used for measuring the experimental group and the control group for testing2O2The pressure on the sheets was 10N each.
The test results of the experimental group and the control group are shown in fig. 4. As can be seen from fig. 4, the impedance of the control group is higher when the carbon paper is introduced than the experimental group, which indicates that after one more component is introduced, the component may interfere with the catalyst performance test, so that the catalyst effect cannot be accurately reflected.
Secondly, the target reactant Li with uniform composition with the catalyst with flat end surfaces in the experimental group2O2The two different points (point A and point B) on the sheet were tested differently, and after the carbon paper was introduced into the control group, the test was similar to Li2O2Two different points (A) on the carbon paper of sheet contact1Points and B1Point) test, and the results of the two points in the experimental group are basically consistent, which may be that the catalyst is not uniformly coated on the carbon paper, so that the catalyst may not completely contact with the reactant in the test surface of the Pt planar electrode. It is shown that when the catalyst is loaded on carbon paper for testing, the coating uniformity is difficult to ensure, and the related performance test is interfered.
Example 2
The end of the Au microelectrode with the diameter of 25 μm is placed in hot aqua regia at 100 ℃ for soaking for 20min, the Au microelectrode is rotated at a constant speed while soaking (the Au microelectrode is kept to rotate at a constant speed in the axial direction, the rotating speed is 10 r/min), and then the corrosion depth is about 4 μm under an optical microscope. Then, the probe was ultrasonically washed 3 times with ethanol and dried to obtain an Au probe having a pore with an etching depth of about 4 μm at the end.
Then grinding the prepared RuO2The powder (particle size 40nm) was filled into the etched Au probe, and filling was confirmed under an optical microscope. Next, the Au probe was placed on the SECM stage and the Au probe was adjusted downward until it was tightly held against Li placed on a quartz glass wafer2O2Sheet, and subjected to LSV test (Linear Scan)Voltammetry), the results are shown in fig. 5.
The above LSV test was performed in 0.5M LiTFSI TEGDME electrolyte, with a platinum wire as the counter electrode, a silver wire as the reference, and an Au probe as the working electrode. During testing, the wire clamps for LSV testing are respectively clamped on the corresponding electrodes.
As can be seen from FIG. 5, a current appears at about 0.4V, demonstrating RuO2Start catalyzing Li at a voltage of about 0.4V2O2And as the voltage is increased, more and more energy is supplied to the catalytic reaction, the charge transfer is faster and faster, and the current is gradually increased. When the voltage is increased to about 0.8V, the current of the catalytic reaction tends to rise linearly, and at the moment, the RuO catalyst2The electrolyte may be catalytically decomposed, and since the catalytic reactant is carried out in the electrolyte, the supply amount of the electrolyte is large, which can cause the catalytic current to rapidly increase. From FIG. 5, RuO can be derived2Catalytic Li2O2The preferable voltage of the reaction is 0.4-0.8V, and the voltage can be adjusted in the interval to obtain the corresponding catalytic reaction current.
Claims (10)
1. A method for characterizing catalyst performance based on an improved SECM probe, comprising: and mounting the improved SECM probe filled with the catalyst powder to be detected on a scanning electrochemical microscope, pressing the probe on the solid reactant, and performing electrochemical performance characterization on the catalyst-catalyzed solid reactant.
2. The method of characterizing catalyst performance of claim 1, wherein the catalyst is electrochemically characterized using one of impedance testing, linear sweep voltammetry.
3. The method of claim 1, wherein the modified SECM probe is a microelectrode terminated with a hole to receive the catalyst powder to be detected.
4. The method for characterizing catalyst performance according to claim 3, wherein the diameter of the metal wire in the micro-electrode is 5 to 100 μm.
5. The method for characterizing the performance of the catalyst according to claim 1, wherein the particle size of the catalyst powder is 2 to 200 nm.
6. The method of claim 1, wherein the modified SECM probe is prepared by the method of:
and corroding the end part of the microelectrode, forming a pore for containing the powder to be detected in the microelectrode, and performing post-treatment to obtain the improved SECM probe.
7. The method for characterizing the performance of the catalyst according to claim 6, wherein hot aqua regia or concentrated hydrochloric acid is used as an etching solution when the microelectrode is etched;
when hot aqua regia is used, the corrosion temperature is 100 ℃.
8. The method of claim 3 or 6, wherein when the catalyst powder is loaded into the pores, whether the pores are filled is observed using an optical microscope.
9. The method of claim 6, wherein the microelectrodes are maintained in constant axial rotation during the etching of the microelectrodes.
10. The method of claim 1 wherein the modified SECM probe is provided with a pressure sensor that monitors and adjusts the pressure at which the modified SECM probe is pressed against the solid reactant.
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