CN217359597U - Dual-functional reaction device for solid-liquid phase in-situ infrared detection - Google Patents

Dual-functional reaction device for solid-liquid phase in-situ infrared detection Download PDF

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CN217359597U
CN217359597U CN202220919980.5U CN202220919980U CN217359597U CN 217359597 U CN217359597 U CN 217359597U CN 202220919980 U CN202220919980 U CN 202220919980U CN 217359597 U CN217359597 U CN 217359597U
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gas diffusion
slot
diffusion electrode
base
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徐延志
薄烁文
程位任
刘庆华
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University of Science and Technology of China USTC
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Abstract

The utility model discloses a solid-liquid phase normal position infrared detection uses difunctional reaction unit, relate to spectroelectrochemistry detection technical field, difunctional reaction unit includes the base, the base sets firmly the cell body, be equipped with working electrode between base and the cell body, the cell body sets firmly the upper cover plate, be equipped with the installation pole that is used for the synchrotron radiation infrared light to pass through on the upper cover plate, the last gas diffusion electrode that is equipped with of working electrode, the both sides fastening of gas diffusion electrode is equipped with the polytetrafluoroethylene gasket, the gas diffusion electrode includes gas diffusion electrode PTEE layer, gas diffusion electrode carbon-layer and catalyst layer, be equipped with the gas diffusion electrode carbon-layer on the gas diffusion electrode PTEE layer in proper order, the catalyst layer. The utility model discloses difunctional reaction unit, through plane infrared window and gas diffusion electrode gasket design, adjustment gasket thickness reaches the micron order and can realize the good coupling with the infrared test port of synchrotron radiation, utilizes the high luminance of synchrotron radiation infrared light source at the micro-zone, high flux, high collimation characteristic.

Description

Dual-functional reaction device for solid-liquid phase in-situ infrared detection
Technical Field
The utility model relates to a spectrum electrochemistry detects technical field, specifically is a solid-liquid phase normal position infrared detection uses difunctional reaction unit.
Background
The infrared spectrum technology can detect the inherent molecular vibration of the catalyst surface interface functional group, provides rich surface interface chemical information, has simple and quick test method, does not need marking or carrying out damaging pretreatment on a sample, and is widely applied to the in-situ characterization of the heterogeneous catalysis mechanism research. In the in-situ electrochemical-infrared spectrum detection process, because the liquid-phase electrolyte seriously weakens the infrared signal intensity and the adsorption and re-adsorption interference of gas/solid/liquid multiphase complex products exists under the working condition, the method puts an extremely high requirement on the detection sensitivity of the infrared spectrum.
The in-situ electrochemical cell in the existing detection equipment has high processing difficulty, the application range of the detection device is limited by the diversity of samples and electrolyte, and the detection has repeatability. The existing thin-layer flow electrochemical cell design is also used for reducing secondary adsorption interference and improving the signal-to-noise ratio, but only gas can be dissolved in electrolyte for reaction, because the gas solubility is low, the reaction efficiency is low.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a solid-liquid phase normal position infrared detection uses difunctional reaction unit, difunctional reaction unit can make full use of synchrotron radiation infrared light source advantage, simulates real electrochemical process, and assembly and disassembly is convenient, and detection method is simple.
The purpose of the utility model can be realized by the following technical scheme:
the utility model provides a difunctional reaction unit is used in infrared detection of solid-liquid phase normal position, difunctional reaction unit includes the base, and the cell body is fastened to the base, is equipped with working electrode between base and the cell body, and the cell body is fastened and is equipped with the upper cover plate, is equipped with the installation pole that is used for synchrotron radiation infrared light to pass through on the upper cover plate, is equipped with the gas diffusion electrode on the working electrode, and the both sides fastening of gas diffusion electrode is equipped with the polytetrafluoroethylene gasket.
The gas diffusion electrode comprises a gas diffusion electrode PTEE layer, a gas diffusion electrode carbon layer and a catalyst layer, wherein the gas diffusion electrode PTEE layer is sequentially provided with the gas diffusion electrode carbon layer and the catalyst layer.
Further, one side of base is equipped with the gas pump and goes into the slot, and the other end is equipped with the gas pump and goes out the slot, lies in centre of a circle department on the base and is equipped with the round hole of going into slot, gas pump and go out the slot intercommunication with the gas pump, is equipped with the first through-hole of array distribution on the base, and the base is connected with the cell body block, and cell body, base, working electrode, upper cover plate, gas diffusion electrode pass through bolted connection.
Furthermore, one end of the tank body is provided with a liquid storage groove, the other end of the tank body is provided with a rectangular hole, second through holes distributed in an array mode are formed in the rectangular hole, fastening bolts are arranged on the second through holes, through holes communicated with the rectangular hole and the liquid storage groove are formed in the tank body, a groove is formed in the lower end of the tank body, an upper cover plate is arranged in the rectangular hole, and a third through hole is formed in the upper cover plate.
Furthermore, be equipped with the installation pole with upper cover plate threaded connection on the upper cover plate, be equipped with signal channel on the installation pole, the one end fastening of installation pole is equipped with infrared window, forms the electrolyte shallow slot that forms circular planar structure between infrared window and the working electrode, and one side of cell body is equipped with electrolyte pump and goes into the slot, and the other end is equipped with electrolyte pump and goes out the slot, and electrolyte pump goes into the slot, electrolyte pump goes out the slot and holds the liquid recess intercommunication.
Further, the gas diffusion electrode is hydrophobic carbon cloth.
Furthermore, a first electrode slot and a second electrode slot are arranged on the cell body, a reference electrode is connected onto the first electrode slot, a counter electrode is connected onto the second electrode slot, the first electrode slot is communicated with the electrolyte pump-in slot, the second electrode slot is communicated with the electrolyte pump-out slot, and the reference electrode and the counter electrode are connected with an external electrochemical working platform.
Further, the fastening bolt penetrates through the third through hole, the second through hole, the gas diffusion electrode and the first through hole in the base.
The utility model has the advantages that:
1. the utility model discloses difunctional reaction unit, through plane infrared window and gas diffusion electrode gasket design, good coupling with synchrotron radiation infrared test port can be realized to adjustment gasket thickness reaching the micron order, can make full use of synchrotron radiation infrared light source high brightness in the micro-area, high flux, high collimation characteristic, carbon cloth also is favorable to infrared signal's outgoing simultaneously, is convenient for the detector to receive effective signal, obtains the infrared spectroscopy signal of high SNR;
2. the utility model discloses difunctional reaction unit can effectively avoid gas too low in the electrolyte solubility, simulates real gas reduction flow cell electrochemistry detection environment, directly perceivedly distinguishes the reaction midbody in the energy conversion process, is used for the evolution research of the reaction midbody in the normal position research energy conversion process;
3. the utility model discloses difunctional reaction unit, normal position electrochemical cell do not have specific window design, processing low cost, and assembly and disassembly is convenient.
Drawings
The present invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic structural view of the dual-function reaction apparatus of the present invention;
FIG. 2 is a schematic diagram of the working electrode structure of the present invention;
FIG. 3 is a top view of the tank body of the present invention;
fig. 4 is an exploded structural schematic diagram of the reference electrode and the counter electrode of the present invention;
fig. 5 is a schematic diagram of the infrared signal curve of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by a person skilled in the art without making creative efforts belong to the protection scope of the present invention.
A dual-function reaction device for solid-liquid phase in-situ infrared detection is disclosed, as shown in fig. 1 and fig. 3, and comprises a base 2, wherein a round hole is formed in the base 2, the round hole is formed in the center of the base 2, a gas pump is arranged at one side of the base 2 and is pumped into a slot 10, a gas pump is arranged at the other end of the base 2 and is pumped out of the slot 11, the round hole is communicated with the gas pump in the slot 10 and the gas pump out of the slot 11, first through holes distributed in an array mode are formed in the base 2, the first through holes are located at four corners of the base 2, and the first through holes are not shown in the figure.
The base 2 is fixedly provided with the pool body 3, the pool body 3 is made of polyether-ether-ketone resin, the pool body has the advantage of strong alkali resistance, the base 2 is connected with the pool body 3 in a clamping manner, the base 2 is fixedly provided with the working electrode 1, and the working electrode 1 is positioned between the base 2 and the pool body 3.
The one end of cell body 3 is equipped with holds liquid recess 12, and the other end is equipped with the rectangular hole, is equipped with array distribution's second through-hole in the rectangular hole, is equipped with fastening bolt 31 on the second through-hole, is equipped with the through hole on the cell body 3, through hole intercommunication rectangular hole with hold liquid recess 12, be equipped with upper cover plate 4 in the rectangular hole, the four corners department of upper cover plate 4 is equipped with the third through-hole, be equipped with installation pole 5 on the upper cover plate 4, installation pole 5 and 4 threaded connection of upper cover plate are equipped with signal channel 15 on the installation pole 5.
An infrared window 14 is tightly arranged at one end of the mounting rod 5, one end of the mounting rod 5 penetrates through the upper cover plate 4 and is located in the liquid storage groove 12, an electrolyte shallow groove 13 is formed between the infrared window 14 and the working electrode 1, the electrolyte shallow groove 13 is of a circular plane structure, an electrolyte pump inlet slot 8 is arranged on one side of the tank body 3, an electrolyte pump outlet slot 9 is arranged at the other end of the tank body, and the electrolyte pump inlet slot 8, the electrolyte pump outlet slot 9 and the liquid storage groove 12 are communicated.
As shown in fig. 2, a gas diffusion electrode is arranged on the working electrode 1, the gas diffusion electrode is made of hydrophobic carbon cloth, polytetrafluoroethylene gaskets 24 are tightly arranged on two sides of the gas diffusion electrode, the gas diffusion electrode comprises a gas diffusion electrode PTEE layer 21, a gas diffusion electrode carbon layer 22 and a catalyst layer 23, the gas diffusion electrode PTEE layer 21 is sequentially provided with a gas diffusion electrode carbon layer 22 and a catalyst layer 23, and the catalyst layer 23 is sputtered on the gas diffusion electrode carbon layer 22.
As shown in fig. 3, a first electrode slot 34 and a second electrode slot 35 are arranged on the cell body 3, the first electrode slot 34 is connected with a reference electrode 36, the second electrode slot 35 is connected with a counter electrode 37, the first electrode slot 34 is communicated with the electrolyte pump-in slot 8, the second electrode slot 35 is communicated with the electrolyte pump-out slot 9, the reference electrode 36 is an Ag/AgCl reference electrode, the counter electrode 37 is a platinum wire counter electrode, the reference electrode 36 and the counter electrode 37 are firstly sleeved with a sealing ring, and then are respectively inserted into the first electrode slot 34 and the second electrode slot 35 and then screwed, the reference electrode 36 is provided with an external thread 38, the counter electrode 37 is also provided with an external thread 38, and the reference electrode 36 and the counter electrode 37 are connected with an external electrochemical working platform.
The electrolyte is pumped into the guide pipe and pumped out of the guide pipe, the seal rings are sleeved on the guide pipe, then the electrolyte is respectively inserted into the electrolyte pumping slot 8 and the electrolyte pumping slot 9, the threads are screwed for fixation, the electrolyte is pumped into the liquid storage groove 12 through circulation, gas is pumped into the round hole, the lower end of the tank body 3 is provided with a notch, and the notch is used for placing the base 2 and the lead.
Pass third through-hole, second through-hole, gas diffusion electrode and the first through-hole on the base 2 through fastening bolt 31, fixed reaction unit adjusts installation pole 5 on the upper cover plate 4, makes infrared window 14 parallel with the lower surface of cell body 3, forms micron order electrolyte thin layer through the polytetrafluoroethylene gasket 24 of micron thickness between the sample that awaits measuring and the infrared window 14.
When the gas diffusion electrode carbon layer is used, Ag nano particles of a sample to be detected are firstly sputtered on the gas diffusion electrode carbon layer 22, and the specific operation is as follows: weighing 10mg of a powder sample, sequentially adding 30 mu L of liquid, 300 mu L of water and 300 mu L of isopropanol, ultrasonically mixing for 10min uniformly, moving the powder sample into a spray gun spray can by a rubber head dropper, connecting the spray gun with an air pump, adjusting a sample outlet of the spray nozzle, sputtering a sample liquid on a 4X 4cm gas diffusion electrode carbon layer 22 by air pressure, drying after sputtering is finished to form a sample layer with the thickness of about 1 mu m, installing a working electrode 1, fixing a base 2/cell body 3 and an upper cover plate 4 by a fastening bolt 31, and installing a reference electrode 36 and a counter electrode 37.
Will synchronize withThe radiation infrared light is focused on the surface of the sample to be detected from the signal channel 15, and the infrared spectrum is collected as a primary background spectrum. Starting a circulating pump in an external circulating device to mix the 1M KOH electrolyte and the high-purity CO 2 And respectively pumping gas into the liquid storage groove 12 and the circular hole to form stable circulating electrolyte and atmosphere, refocusing the synchrotron radiation infrared light on the surface of the sample to be detected, and collecting the infrared spectrum as a secondary background spectrum by taking the primary background spectrum as a background. Adjusting the mounting rod 5 to control the thickness of an electrolyte film between the infrared window 14 and a sample to be detected, enabling the thickness to be in a micron order, refocusing synchrotron radiation infrared light on the surface of the sample to be detected, collecting infrared spectrum as a third background spectrum by taking a second background spectrum as a background, respectively connecting leads of the reference electrode 36, the counter electrode 37 and the working electrode 1 with an external electrochemical working platform, setting potential and scanning time after electrification, modifying electrochemical detection parameters after electrochemical signals of the sample to be detected are stabilized, and collecting electrochemical data.
In order to detect infrared spectrum signals under the electrochemical working condition, a constant potential method is adopted in the example, and the voltages are respectively fixed as follows: rhe at 0.1V and 0.5V vs. 1min under applied voltage, and infrared spectral acquisition was performed against a background of three background spectra.
As shown in FIG. 5, a wave number of 1976cm has been observed at a voltage of 0.1V -1 And-2024 cm -1 Two infrared signal peaks appear, possibly corresponding to the reaction intermediate product CO respectively bridge And CO atop And when the voltage is 0.5V, the intensity of the infrared signal peak is increased, which shows that the infrared signal peak corresponds to a reaction intermediate product of the sample to be detected in the electrochemical process. To verify the above conclusions, the CO can also be used 2 The atmosphere being isotopically substituted, e.g. by
Figure BDA0003605505840000061
Atmosphere change to
Figure BDA0003605505840000062
By performing the same operation as above, other adsorbed infrared signal peaks can be excluded according to the appearance position and displacement of the infrared signal peak of the isotope with the applied voltageFurther, the structure of the reaction intermediate product is clarified, and the evolution of the reaction intermediate product is inferred.
In the description herein, references to the description of "one embodiment," "an example," "a specific example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above embodiments, and that the foregoing embodiments and descriptions are provided only to illustrate the principles of the present invention without departing from the spirit and scope of the present invention.

Claims (7)

1. A difunctional reaction device for solid-liquid phase in-situ infrared detection is characterized by comprising a base (2), a pool body (3) is fixedly arranged on the base (2), a working electrode (1) is arranged between the base (2) and the pool body (3), an upper cover plate (4) is fixedly arranged on the pool body (3), an installation rod (5) for synchronously radiating infrared light to pass through is arranged on the upper cover plate (4), a gas diffusion electrode is arranged on the working electrode (1), and polytetrafluoroethylene gaskets (24) are fixedly arranged on two sides of the gas diffusion electrode;
the gas diffusion electrode comprises a gas diffusion electrode PTEE layer (21), a gas diffusion electrode carbon layer (22) and a catalyst layer (23), wherein the gas diffusion electrode carbon layer (22) and the catalyst layer (23) are sequentially arranged on the gas diffusion electrode PTEE layer (21).
2. The dual-function reaction device for solid-liquid phase in-situ infrared detection as claimed in claim 1, wherein one side of the base (2) is provided with a gas pumping insertion slot (10), the other end of the base is provided with a gas pumping insertion slot (11), a circular hole communicated with the gas pumping insertion slot (10) and the gas pumping insertion slot (11) is arranged at the center of a circle on the base (2), the base (2) is provided with first through holes distributed in an array manner, the base (2) is connected with the cell body (3) in a clamping manner, and the cell body (3), the base (2), the working electrode (1), the upper cover plate (4) and the gas diffusion electrode are connected through bolts.
3. The dual-function reaction device for solid-liquid phase in-situ infrared detection as claimed in claim 2, wherein one end of the tank body (3) is provided with a liquid storage groove (12), the other end is provided with a rectangular hole, the rectangular hole is provided with second through holes distributed in an array, the second through holes are provided with fastening bolts (31), the tank body (3) is provided with through holes communicating the rectangular hole and the liquid storage groove (12), the lower end of the tank body (3) is provided with a slot, the rectangular hole is provided with an upper cover plate (4), and the upper cover plate (4) is provided with a third through hole.
4. The dual-function reaction device for solid-liquid phase in-situ infrared detection as claimed in claim 3 is characterized in that a mounting rod (5) in threaded connection with the upper cover plate (4) is arranged on the upper cover plate (4), a signal channel (15) is arranged on the mounting rod (5), an infrared window (14) is tightly arranged at one end of the mounting rod (5), an electrolyte shallow groove (13) of a circular plane structure is formed between the infrared window (14) and the working electrode (1), an electrolyte pumping slot (8) is arranged at one side of the tank body (3), an electrolyte pumping slot (9) is arranged at the other end of the tank body, and the electrolyte pumping slot (8), the electrolyte pumping slot (9) and the liquid storage groove (12) are communicated.
5. The dual-function reaction device for in-situ infrared detection of solid and liquid phases as claimed in claim 1, wherein the gas diffusion electrode is a hydrophobic carbon cloth.
6. The dual-function reaction device for solid-liquid phase in-situ infrared detection according to claim 2, wherein a first electrode slot (34) and a second electrode slot (35) are arranged on the cell body (3), the first electrode slot (34) is connected with a reference electrode (36), the second electrode slot (35) is connected with a counter electrode (37), the first electrode slot (34) is communicated with the electrolyte pump-in slot (8), the second electrode slot (35) is communicated with the electrolyte pump-out slot (9), and the reference electrode (36) and the counter electrode (37) are connected with an external electrochemical working platform.
7. The dual-function reaction device for solid-liquid phase in-situ infrared detection as claimed in claim 3 is characterized in that a fastening bolt (31) passes through the third through hole, the second through hole, the gas diffusion electrode and the first through hole on the base (2).
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