CN109374535A - A kind of electrochemical experimental device for spectral measurement - Google Patents
A kind of electrochemical experimental device for spectral measurement Download PDFInfo
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- CN109374535A CN109374535A CN201811220426.2A CN201811220426A CN109374535A CN 109374535 A CN109374535 A CN 109374535A CN 201811220426 A CN201811220426 A CN 201811220426A CN 109374535 A CN109374535 A CN 109374535A
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- 230000003595 spectral effect Effects 0.000 title claims abstract description 15
- 238000005259 measurement Methods 0.000 title claims abstract description 14
- 230000003287 optical effect Effects 0.000 claims abstract description 38
- 230000005540 biological transmission Effects 0.000 claims abstract description 23
- 239000003990 capacitor Substances 0.000 claims abstract description 22
- 238000001228 spectrum Methods 0.000 claims abstract description 15
- 239000004065 semiconductor Substances 0.000 claims abstract description 9
- 230000005611 electricity Effects 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 238000001514 detection method Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 abstract description 8
- 238000002848 electrochemical method Methods 0.000 abstract description 4
- 230000005518 electrochemistry Effects 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 3
- 238000000149 argon plasma sintering Methods 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 206010044565 Tremor Diseases 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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- G—PHYSICS
- 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
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Abstract
The present invention relates to photochemistry and electrochemical fields, a kind of electrochemical experimental device for spectral measurement, including high-voltage DC power supply, charging resistor, charging cable, spark switch, capacitor, power divider, attenuator, transmission line I, oscillograph, transmission line II, bracket, sample cavity, optical tester, thermometer, semiconductor cooler, thermally conductive and potentiostat, sample cavity is compact-sized, and balance the demand of electrochemistry experiment and spectrum experiment, electrode with light reflection function makes the diffusion path of light shorter, light scattering is lower, the signal-to-noise ratio of spectrum improves；Voltage pulse generative circuit and compact-sized sample cavity with special designing, it can be after carrying out high voltage processing to sample, the electrochemical properties and spectral characteristic of study sample simultaneously, the high-voltage pulse rule being applied on sample is stablized, the signal-to-noise ratio of obtained spectrum improves, high-voltage pulse generative circuit is relatively simple, can apply high voltage to sample and carry out spectrum and electrochemical measurement.
Description
Technical field
High voltage can be applied to sample the present invention relates to photochemistry and electrochemical field, especially one kind and carry out spectrum
And a kind of electrochemical experimental device for spectral measurement of electrochemical measurement.
Background technique
Electrochemistry is combined with spectroscopy can be used in the active substance of redox reaction, and usual sample is located at electric
Chemistry is intracavitary, and uses laser irradiation sample, studies the characteristic of reaction by light that sample reflects using optical tester record,
Spectral acquisition times in the prior art in the measurement of certain reactions are longer, and need to be independent for every kind of redox reaction
Prepare different samples.It is needed to apply in the reaction that high voltage just can be carried out some, especially is needing to apply high-voltage pulse
In the case where, switch needs to be switched fast between opening and closing state, usually when discharge switch is opened, charging current meeting
Flow to discharge circuit from high-voltage DC power supply, this electric current need the regular hour could complete attenuation be zero, this can hinder to hold
Pass comes back to closed state, and the prior art avoids above-mentioned phenomenon using special gas or specially designed construction of switch, but
It is this meeting so that the structure of device becomes complicated, and operating process is cumbersome, inappropriate experimental implementation can generate irregular shakiness
Fixed voltage pulse, a kind of electrochemical experimental device for spectral measurement are able to solve problem.
Summary of the invention
To solve the above-mentioned problems, the present invention has novel voltage pulse generative circuit, and using the sample of special designing
Product chamber makes it possible to after carrying out high voltage processing to sample, while the electrochemical properties and spectral characteristic of study sample.
The technical scheme adopted by the invention is that:
A kind of electrochemical experimental device for spectral measurement include high-voltage DC power supply, charging resistor, charging cable,
Spark switch, capacitor, power divider, attenuator, transmission line I, oscillograph, transmission line II, bracket, sample cavity, optic test
Instrument, thermometer, semiconductor cooler, thermally conductive and potentiostat, xyz are three-dimensional coordinate system, the high-voltage DC power supply
With output head anode and negative pole of output end, high-voltage DC power supply output voltage range is 1kV to 2kV, the power divider
With input, output end I and output end II, the potentiostat has anode and cathode, the output end II of power divider
Successively cable connection attenuator, transmission line I and oscillograph, the sample cavity, bracket, semiconductor cooler and thermally conductive from upper and
Under be sequentially connected, bracket is connected with thermometer, and the optical tester is located at right above sample cavity, and the optical tester can
Launch laser and spectrum analysis is carried out to the light of collection, the laser includes pump light and detection light；Sample cavity include cavity,
Plane mirror, working electrode, to electrode, washer, sample, transmissive window, chamber lid, reference electrode, connector I and connector II, the plane
Mirror, working electrode are respectively positioned in cavity electrode, washer, sample and transmissive window, and the connector I and connector II of sample cavity connect respectively
The anode and cathode of potentiostat are connect, potentiostat is located at below the sample cavity in bracket, and the output of high-voltage DC power supply is rectified
Pole successively cable connection charging resistor, charging cable, the contact II of spark switch, the rotary shaft of spark switch, capacitor and high straightening
The negative pole of output end in galvanic electricity source；The spark switch includes rotation motor, rotary shaft, horizon bar, trigger electrode I, two contacts
I, trigger electrode II and two contact II, rotary shaft are vertically arranged on rotation motor, and rotary shaft, water are connected among horizon bar
Flat pole length is 120 millimeters, and trigger electrode I and trigger electrode II are the squares that side length is 8 millimeters and are respectively arranged in water
The both ends of flat bar, the rotary shaft, horizon bar, trigger electrode I and trigger electrode II are electrically being connected；Two contact I are axis
The identical metal cylinder of line in the y-direction, 10 millimeters and arranged in co-axial alignment are divided between two contact I, and the metal cylinder is high
Degree is 10 millimeters, basal diameter is 10 millimeters, and the axis of contact I and the axial line distance of rotary shaft are 64 millimeters, two contact II
It is the metal strip of identical 1/6 circular shape, the center of circle of the circular arc is located on the axis of rotary shaft and radius of curvature is 64
Millimeter, two metal strips are 10 millimeters of the direction y interval and in being arranged above and below, and the mutual electricity conducting of two contact I, two are touched
The mutual electricity conducting of point II, rotation motor can make horizon bar rotate in the horizontal plane by rotary shaft, and make triggering electricity
Pole I and trigger electrode II can contactlessly pass through the interval between two contact I and the interval between two contact II；It is described
Cavity is that the cylinder of axis in the y-direction is barrel-shaped, and plane mirror is axis cylinder in the y-direction and is located at cavity bottom, plane mirror
Diameter is made by 30 millimeters and of polytetrafluoroethylene material, and the upper surface of plane mirror and side deposition are prepared with working electrode and right
Electrode, working electrode and is made of gold electrode and with a thickness of 500 microns；Cavity side mask connector I and connects there are two through-hole
Head II can be in close contact by two through-holes and working electrode and to electrode in the side of plane mirror respectively；Washer is by ring
Oxygen resin material is made and is located at the upper surface of plane mirror, and the outer diameter of washer is 30 millimeters, internal diameter is 26 millimeters, thickness representative value
It is 5 to 30 microns, transmissive window is located at the top of washer, and the diameter of transmissive window is 30 millimeters, and sample is placed within the internal diameter of washer,
Chamber lid is installed on above cavity, and chamber lid light transmission and can seal cavity, and chamber lid can be by transmissive window, washer and plane mirror
Between compress, chamber lid and transmissive window all have the via hole in the direction y, and reference electrode can be inserted into sample by the via hole, institute
State reference electrode successively cable connection capacitor, the rotary shaft of spark switch, spark switch contact I, power divider input
End, the output end I of power divider, transmission line II and connector II.
Apply the principle of high voltage pulse to sample:
There are two gaps for the spark switch tool, are respectively used to be charged and discharged, can eliminate in pulse generation circuit
The irregular and unstable pulse generated due to charge electric discharge.The rotation motor of spark switch passes through rotary shaft and horizon bar band
Dynamic trigger electrode I and trigger electrode II rotates in the horizontal plane, so that trigger electrode I and trigger electrode II are in time alternately
Contact I and contact can not be passed through simultaneously by contact I and contact II, and in synchronization, trigger electrode I and trigger electrode II
II, likewise, trigger electrode I and trigger electrode II can not pass through contact II and contact I simultaneously.When trigger electrode I or triggering electricity
When pole II passes through contact II, the gap between trigger electrode I or trigger electrode II and contact II generates spark, so that triggering
Electrode I or trigger electrode II are connected with contact II, and high-voltage DC power supply charges to capacitor；When trigger electrode I or triggering electricity
When pole II passes through contact I, the gap between trigger electrode I or trigger electrode II and contact I generates spark, so that triggering electricity
Pole I or trigger electrode II are connected with contact I, and capacitor discharges to sample in sample cavity.
The principle of electrochemical measurement is carried out to sample:
The anode of the potentiostat passes through connector I respectively with cathode and connects working electrode with connector II and to electrode, with
Electrochemical potential is applied to sample, sample will appear different chemical forms under different electrochemical potentials.
The principle of spectrum experiment measurement is carried out to sample:
The optical tester launches two light pulses, referred to as pump light and detection light, the pump light and detection light
With different power, frequency and duration, detecting light can be adjusted relative to the delay time of pump light, optical tester
The pump light of sending passes sequentially through chamber lid and transmissive window is mapped on sample from top to bottom, so that sample generates reaction, optic test
The detection light that instrument issues passes sequentially through chamber lid and transmissive window is mapped on sample and generates a degree of scattering, and a portion is penetrated
Reflected light is reflected to form to working electrode and to the detection light of electrode top, the reflected light is mapped to sample again from top to bottom
On product, reflected light described in a portion forms secondary transmitted light by sample, and the secondary transmitted light passes sequentially through
Enter optical tester after penetrating window and chamber lid, it, can by analyzing the feature for the secondary transmitted light that optical tester collects
Obtain the correlation properties of sample.
The laser that optical tester is launched and transmissive window upper surface method are mutually in that sample is incident at 0.5 degree of angle, advantage be from
Spatially the light that transmissive window upper surface is reflected is separated with the light after sample effect, so that optical tester be avoided to acquire
To spectrogram in there is the interference of pump light.
Working electrode made of gold using plane mirror upper surface and to electrode as working electrode, rather than as existing skill
Like that using metal grid mesh as working electrode in certain spectral measurement devices of art, advantage is to can be avoided the scattering of light to ask
Topic increases the signal-to-noise ratio of the optical signal of optical tester acquisition, in addition, since light passes twice through sample, so that optic test
The intensity for the signal that instrument collects doubles, and this point is extremely important in the case where sample size is less, and the present invention carries out spectrum
Less sample is only needed when experiment, and the time up to electrochemical equilibrium state then can be reduced to using relatively thin sample, for
Certain quick redox cycle processes are extremely important.
The tectonic sieving of the sample cavity can be suitable for the sample of different-thickness by selecting the washer of different-thickness,
And there is good air-tightness.
It is different according to the specific sample of research, the voltage difference V in following methods step1Range is from 0 to 300mV, voltage difference V2
From 300mV to 800mV, one embodiment is range: for the FePC on the golden substrate surface in oxygen-saturated electrolyte point
Sub- film sample, voltage difference V1For 50mV, voltage difference V2For 350mV.
The step of being tested using a kind of electrochemical experimental device for spectral measurement are as follows:
Step 1, by sample be added sample cavity in, by chamber lid install to cavity and make transmissive window, washer and plane mirror it
Between compress；
Step 2, high-voltage DC power supply is opened, by charging resistor and charging cable output voltage to spark switch, opens rotation
Turn motor, the range of speeds of rotation motor is 1000 to 5000 revs/min, and spark switch periodically makes capacitor and high straightening
The conducting of galvanic electricity source or capacitor are connected with sample cavity, and high-voltage DC power supply is to capacitor charging and capacitor to two mistakes of sample cavity discharging
Journey alternately, continues 5 minutes；
Step 3, high-voltage DC power supply is closed, rotation motor is closed；
Step 4, optical tester is opened, the laser for launching optical tester and transmissive window upper surface normal direction are at 0.5
It is incident to spend angle, and is mapped on sample, the energy range of each pumping light pulse is 4mJ to 8mJ, the duration is 1 picosecond, each
The energy range of detecting optical pulses is 0.5mJ to 1mJ, the duration is 800 femtoseconds, and detecting optical pulses are relative to pumping light pulse
Time delay be 2 to 5 picoseconds；
Step 5, adjust potentiostat so that working electrode and to the voltage difference between electrode be V1, voltage difference V1Range from
0 arrives 300mV, and to apply electrochemical potential to sample, so that occurring the first chemical form in sample, optical tester is collected anti-
Light is penetrated, continues 2 minutes；
Step 6, adjust potentiostat so that working electrode and to the voltage difference between electrode be V2, voltage difference V2Range from
300mV to 800mV, to apply electrochemical potential to sample, so that occurring second of chemical form in sample, optical tester is received
Collect reflected light, continues 2 minutes；
Step 7, repeat above-mentioned steps 5 and step 6, the repetition is carried out continuously ten times, optical tester is collected
Obtained reflected light information is handled and is averaged, and the difference light of the first chemical form of sample and second of chemical form is obtained
Spectrum.
The beneficial effects of the present invention are:
Sample cavity in the present invention is compact-sized, and balances the demand of electrochemistry experiment and spectrum experiment, has light anti-
The electrode for penetrating function makes the diffusion path of light shorter, and light scattering is lower, and the signal-to-noise ratio of spectrum improves, in addition, high-voltage pulse is raw
Relatively simple at circuit, the high-voltage pulse being applied on sample more rule is stablized.
Detailed description of the invention
It is further illustrated below with reference to figure of the invention:
Fig. 1 is schematic diagram of the present invention；
Fig. 2 is spark switch enlarged diagram；Fig. 3 is the top view of Fig. 2；
Fig. 4 is sample cavity enlarged diagram；Fig. 5 is the A-A cross-sectional view of Fig. 4.
In figure, 1. high-voltage DC power supplies, 2. charging resistors, 3. charging cables, 4. spark switch, 4-1. rotation motor, 4-2.
Rotary shaft, 4-3. horizon bar, 4-4. trigger electrode I, 4-5. contact I, 4-6. trigger electrode II, 4-7. contact II, 5. capacitors, 6.
Power divider, 7. attenuators, 8. transmission line I, 9. oscillographs, 10. transmission line II, 11. brackets, 12. sample cavities, 12-1. chamber
Body, 12-2. plane mirror, 12-3. working electrode, 12-4. is to electrode, 12-5. washer, 12-6. sample, 12-7. transmissive window, 12-
8. chamber lid, 12-9. reference electrode, 12-10. connector I, 12-11. connector II, 13. optical testers, 14. thermometers, 15. half lead
Chiller, 16. thermally conductive, 17. potentiostats.
Specific embodiment
If Fig. 1 is schematic diagram of the present invention, xyz is three-dimensional coordinate system, if Fig. 2 is spark switch enlarged diagram, such as
Fig. 3 is the top view of Fig. 2, including high-voltage DC power supply (1), charging resistor (2), charging cable (3), spark switch (4), capacitor
(5), power divider (6), attenuator (7), transmission line I (8), oscillograph (9), transmission line II (10), bracket (11), sample cavity
(12), optical tester (13), thermometer (14), semiconductor cooler (15), thermally conductive (16) and potentiostat (17), it is described
High-voltage DC power supply (1) has output head anode and negative pole of output end, and high-voltage DC power supply (1) output voltage range arrives for 1kV
2kV, the power divider (6) have input, output end I and output end II, the potentiostat (17) have anode and
Cathode, the output end II of power divider (6) successively cable connection attenuator (7), transmission line I (8) and oscillograph (9) are described
Sample cavity (12), bracket (11), semiconductor cooler (15) and thermally conductive (16) are sequentially connected from top to bottom, bracket (11) connection
Have thermometer (14), the optical tester (13) is located at right above sample cavity (12), and the optical tester (13) can be sent out
It projects laser and spectrum analysis is carried out to the light of collection, the laser includes pump light and detection light；High-voltage DC power supply (1)
Output head anode successively cable connection charging resistor (2), charging cable (3), spark switch (4) contact II (4-7), spark switch
(4) negative pole of output end of rotary shaft (4-2), capacitor (5) and high-voltage DC power supply (1)；The spark switch (4) includes rotation
Motor (4-1), rotary shaft (4-2), horizon bar (4-3), trigger electrode I (4-4), two contact I (4-5), trigger electrode II (4-
6) it is vertically arranged on rotation motor (4-1) with two contact II (4-7), rotary shaft (4-2), connection among horizon bar (4-3)
In rotary shaft (4-2), horizon bar (4-3) length is 120 millimeters, and trigger electrode I (4-4) and trigger electrode II (4-6) are sides
A length of 8 millimeters of square and the both ends for being respectively arranged in horizon bar (4-3), the rotary shaft (4-2), horizon bar (4-3),
Trigger electrode I (4-4) and trigger electrode II (4-6) are electrically being connected；Two contact I (4-5) are axis in the y-direction identical
Metal cylinder, be divided into 10 millimeters and arranged in co-axial alignment between two contact I (4-5), the metal cylinder height is 10 millimeters,
Basal diameter is 10 millimeters, and the axis of contact I (4-5) and the axial line distance of rotary shaft (4-2) are 64 millimeters, two contact II
(4-7) is the metal strip of identical 1/6 circular shape, and the center of circle of the circular arc is located on the axis of rotary shaft (4-2) and song
Rate radius is 64 millimeters, and for two metal strips 10 millimeters of the direction y interval and in being arranged above and below, two contact I (4-5) are mutual
Electricity conducting, electricity conducting, rotation motor (4-1) can make level by rotary shaft (4-2) to two contact II (4-7) mutually
Bar (4-3) rotates in the horizontal plane, and makes trigger electrode I (4-4) and trigger electrode II (4-6) can be contactlessly by two
The interval between interval and two contact II (4-7) between a contact I (4-5).
If Fig. 4 is sample cavity enlarged diagram, Fig. 5 is the A-A cross-sectional view of Fig. 4, sample cavity (12) include cavity (12-1),
Plane mirror (12-2), working electrode (12-3), to electrode (12-4), washer (12-5), sample (12-6), transmissive window (12-7),
Chamber lid (12-8), reference electrode (12-9), connector I (12-10) and connector II (12-11), the plane mirror (12-2), work electricity
Pole (12-3) is respectively positioned on electrode (12-4), washer (12-5), sample (12-6) and transmissive window (12-7) in cavity (12-1)；
The reference electrode (12-9) successively cable connection capacitor (5), the rotary shaft (4-2) of spark switch (4), spark switch (4)
Contact I (4-5), the input terminal of power divider (6), the output end I of power divider (6), transmission line II (10) and connector II
(12-11), the connector I (12-10) and connector II (12-11) of sample cavity (12) are separately connected the positive and negative of potentiostat (17)
Pole, potentiostat (17) are located at below the sample cavity (12) in bracket (11)；The cavity (12-1) is the circle of axis in the y-direction
Column is barrel-shaped, and plane mirror (12-2) is axis cylinder in the y-direction and is located at the bottom cavity (12-1), plane mirror (12-2) diameter
It is made by 30 millimeters and of polytetrafluoroethylene material, the upper surface of plane mirror (12-2) and side deposition are prepared with working electrode
It (12-3) and is made of gold to electrode (12-4), working electrode (12-3) and to electrode (12-4) and with a thickness of 500 microns；Chamber
There are two through-holes for the body side (12-1) tool, and connector I (12-10) and connector II (12-11) can pass through two through-holes respectively
It is in close contact with working electrode (12-3) and to electrode (12-4) in the side of plane mirror (12-2)；Washer (12-5) is by asphalt mixtures modified by epoxy resin
Rouge material is made and is located at the upper surface of plane mirror (12-2), and the outer diameter of washer (12-5) is 30 millimeters, internal diameter is 26 millimeters, thick
Spending representative value is 5 to 30 microns, and transmissive window (12-7) is located at the top of washer (12-5), and the diameter of transmissive window (12-7) is 30 millis
Rice, sample (12-6) are placed within the internal diameter of washer (12-5), and chamber lid (12-8) is installed on above cavity (12-1), chamber lid (12-
8) light transmission and cavity (12-1) can be sealed, chamber lid (12-8) can be by transmissive window (12-7), washer (12-5) peace
It is compressed between face mirror (12-2), chamber lid (12-8) and transmissive window (12-7) all have the via hole in the direction y, reference electrode (12-9) energy
Enough by via hole insertion sample (12-6).
A kind of electrochemical experimental device for spectral measurement include high-voltage DC power supply (1), charging resistor (2),
Charging cable (3), capacitor (5), power divider (6), attenuator (7), transmission line I (8), oscillograph (9), passes spark switch (4)
Defeated line II (10), sample cavity (12), optical tester (13), thermometer (14), semiconductor cooler (15), is led at bracket (11)
Thermal station (16) and potentiostat (17), xyz are three-dimensional coordinate system, and the high-voltage DC power supply (1) has output head anode
And negative pole of output end, high-voltage DC power supply (1) output voltage range are 1kV to 2kV, the power divider (6) has input
End, output end I and output end II, the potentiostat (17) have anode and a cathode, the output end II of power divider (6) according to
Secondary cable connection attenuator (7), transmission line I (8) and oscillograph (9), the sample cavity (12), bracket (11), semiconductor refrigerating
Device (15) and thermally conductive (16) are sequentially connected from top to bottom, and bracket (11) is connected with thermometer (14), the optical tester
(13) it is located at right above sample cavity (12), the optical tester (13) can launch laser and carry out spectrum to the light of collection
Analysis, the laser include pump light and detection light；Sample cavity (12) includes cavity (12-1), plane mirror (12-2), work electricity
Pole (12-3), to electrode (12-4), washer (12-5), sample (12-6), transmissive window (12-7), chamber lid (12-8), reference electrode
(12-9), connector I (12-10) and connector II (12-11), the plane mirror (12-2), working electrode (12-3), to electrode (12-
4), washer (12-5), sample (12-6) and transmissive window (12-7) are respectively positioned in cavity (12-1), the connector I of sample cavity (12)
(12-10) and connector II (12-11) are separately connected the anode and cathode of potentiostat (17), and potentiostat (17) is located at bracket
(11) below sample cavity (12) in, the output head anode of high-voltage DC power supply (1) successively cable connection charging resistor (2), fill
Electric wire (3), the contact II (4-7) of spark switch (4), the rotary shaft (4-2) of spark switch (4), capacitor (5) and high voltage direct current
The negative pole of output end in source (1)；The spark switch (4) includes rotation motor (4-1), rotary shaft (4-2), horizon bar (4-3), touching
Power generation pole I (4-4), two contact I (4-5), trigger electrode II (4-6) and two contact II (4-7), rotary shaft (4-2) are vertical
It is installed on rotation motor (4-1), is connected to rotary shaft (4-2) among horizon bar (4-3), horizon bar (4-3) length is 120 millis
Rice, trigger electrode I (4-4) and trigger electrode II (4-6) are the squares that side length is 8 millimeters and are respectively arranged in horizon bar
The both ends of (4-3), the rotary shaft (4-2), horizon bar (4-3), trigger electrode I (4-4) and trigger electrode II (4-6) are in electricity
Upper conducting；Two contact I (4-5) are the identical metal cylinder of axis in the y-direction, and 10 millis are divided between two contact I (4-5)
Rice and arranged in co-axial alignment, the metal cylinder height is 10 millimeters, basal diameter is 10 millimeters, the axis of contact I (4-5) and rotation
The axial line distance of shaft (4-2) is 64 millimeters, and two contact II (4-7) are the metal strip of identical 1/6 circular shape, described
The center of circle of circular arc is located on the axis of rotary shaft (4-2) and radius of curvature is 64 millimeters, and two metal strips are between the direction y
Every 10 millimeters and in being arranged above and below, the electricity conducting mutually of two contact I (4-5), electricity is connected two contact II (4-7) mutually,
Rotation motor (4-1) can make horizon bar (4-3) rotate in the horizontal plane by rotary shaft (4-2), and make trigger electrode I
(4-4) and trigger electrode II (4-6) can contactlessly pass through interval and the two contact II (4- between two contact I (4-5)
7) interval between；The cavity (12-1) is that the cylinder of axis in the y-direction is barrel-shaped, plane mirror (12-2) be axis in the y-direction
Cylinder and be located at the bottom cavity (12-1), plane mirror (12-2) diameter is made by 30 millimeters and of polytetrafluoroethylene material,
The upper surface of plane mirror (12-2) and side deposition are prepared with working electrode (12-3) and to electrode (12-4), working electrode (12-
3) it and to electrode (12-4) is made of gold and with a thickness of 500 microns；There are two through-hole, connector I for the cavity side (12-1) tool
(12-10) and connector II (12-11) can be respectively by two through-holes and working electrode (12-3) and to electrode (12-4)
It is in close contact in the side of plane mirror (12-2)；Washer (12-5) is made of epoxide resin material and positioned at plane mirror (12-2)
Upper surface, the outer diameter of washer (12-5) is 30 millimeters, internal diameter is 26 millimeters, thickness representative value is 5 to 30 microns, transmissive window (12-
7) it is located at the top of washer (12-5), the diameter of transmissive window (12-7) is 30 millimeters, and sample (12-6) is placed in washer (12-5)
Within internal diameter, chamber lid (12-8) is installed on above cavity (12-1), and chamber lid (12-8) being capable of light transmission and can be by cavity (12-1)
Sealing, chamber lid (12-8) can will compress between transmissive window (12-7), washer (12-5) and plane mirror (12-2), chamber lid (12-8)
The via hole in the direction y is all had with transmissive window (12-7), reference electrode (12-9) can be inserted into sample (12-6) by the via hole
In, the reference electrode (12-9) successively cable connection capacitor (5), the rotary shaft (4-2) of spark switch (4), spark switch (4)
Contact I (4-5), the input terminal of power divider (6), the output end I of power divider (6), transmission line II (10) and connector
II(12-11)。
Apply the principle of high voltage pulse to sample (12-6):
There are two gaps for spark switch (4) tool, are respectively used to be charged and discharged, can eliminate pulse generation circuit
In due to charge electric discharge generate irregular and unstable pulse.The rotation motor (4-1) of spark switch (4) passes through rotary shaft
(4-2) and horizon bar (4-3) drive trigger electrode I (4-4) and trigger electrode II (4-6) to rotate in the horizontal plane, so that triggering
Electrode I (4-4) and trigger electrode II (4-6) alternately pass through contact I (4-5) and contact II (4-7) in time, and same
Moment, trigger electrode I (4-4) and trigger electrode II (4-6) can not pass through contact I (4-5) and contact II (4-7) simultaneously, equally
, trigger electrode I (4-4) and trigger electrode II (4-6) can not pass through contact II (4-7) and contact I (4-5) simultaneously.Work as triggering
When electrode I (4-4) or trigger electrode II (4-6) passes through contact II (4-7), trigger electrode I (4-4) or trigger electrode II (4-6)
Gap between contact II (4-7) generates spark, so that trigger electrode I (4-4) or trigger electrode II (4-6) and contact
II (4-7) conducting, high-voltage DC power supply (1) charge to capacitor (5)；As trigger electrode I (4-4) or trigger electrode II (4-
6) when passing through contact I (4-5), the gap between trigger electrode I (4-4) or trigger electrode II (4-6) and contact I (4-5) is generated
Spark, so that trigger electrode I (4-4) or trigger electrode II (4-6) and contact I (4-5) are connected, capacitor (5) is to sample cavity
(12) sample (12-6) discharges in.
The principle of electrochemical measurement is carried out to sample (12-6):
The anode and cathode of the potentiostat (17) pass through connector I (12-10) and connector II (12-11) connection work respectively
Make electrode (12-3) and to electrode (12-4), to apply electrochemical potential to sample (12-6), sample (12-6) is in different electricity
It will appear different chemical forms under chemical potential.
The principle of spectrum experiment measurement is carried out to sample (12-6):
The optical tester (13) launches two light pulses, referred to as pump light and detection light, the pump light and spy
Surveying light has different power, frequency and duration, and detection light can be adjusted relative to the delay time of pump light, and optics is surveyed
The pump light that examination instrument (13) issues passes sequentially through chamber lid (12-8) and transmissive window (12-7) is mapped to from top to bottom on sample (12-6),
So that sample (12-6) generates reaction, the detection light that optical tester (13) issues passes sequentially through chamber lid (12-8) and transmissive window
(12-7) is mapped on sample (12-6) and generates a degree of scattering, and a portion is mapped to working electrode (12-3) and to electricity
The detection light of the upper surface pole (12-4) is reflected to form reflected light, and the reflected light is mapped to sample (12-6) again from top to bottom
On, reflected light described in a portion forms secondary transmitted light by sample (12-6), and the secondary transmitted light is successively led to
It crosses transmissive window (12-7) and chamber lid (12-8) and enters optical tester (13) afterwards, collected by analyzing optical tester (13)
Secondary transmitted light feature, the correlation properties of sample (12-6) can be obtained.
The laser that optical tester (13) is launched mutually is in that sample is incident at 0.5 degree of angle with the upper surface transmissive window (12-7) method
(12-6), advantage are from the light for spatially reflecting the transmissive window upper surface (12-7) and the light point after sample (12-6) effect
From to the interference of pump light occur in the spectrogram for avoiding optical tester (13) from collecting.
Working electrode (12-3) made of gold using the upper surface plane mirror (12-2) and to electrode (12-4) be used as work
Electrode, rather than using metal grid mesh as working electrode as in certain spectral measurement devices of the prior art, advantage is
It can be avoided the scattering problems of light, increase the signal-to-noise ratio of the optical signal of optical tester (13) acquisition, in addition, twice due to light
By sample, so that the intensity for the signal that optical tester (13) collects doubles, this point situation less in sample size
Under it is extremely important, apparatus of the present invention carry out only needing less sample when spectrum experiment, and can then be subtracted using relatively thin sample
The time of electrochemical equilibrium state is reached less, it is extremely important for certain quick redox cycle processes.
The tectonic sieving of the sample cavity (12) can be suitable for difference by selecting the washer (12-5) of different-thickness
The sample of thickness, and there is good air-tightness.
Apparatus of the present invention have the voltage pulse generative circuit and compact-sized sample cavity of special designing, can be to sample
After product carry out high voltage processing, at the same the electrochemical properties and spectral characteristic of study sample, the high-voltage pulse being applied on sample
Rule is stablized, and the signal-to-noise ratio of obtained spectrum improves.
Claims (1)
1. a kind of electrochemical experimental device for spectral measurement, including high-voltage DC power supply (1), charging resistor (2), charging cable
(3), spark switch (4), capacitor (5), power divider (6), attenuator (7), transmission line I (8), oscillograph (9), transmission line II
(10), bracket (11), sample cavity (12), optical tester (13), thermometer (14), semiconductor cooler (15), thermally conductive
(16) and potentiostat (17), xyz are three-dimensional coordinate system, and the high-voltage DC power supply (1) has output head anode and defeated
Outlet cathode, high-voltage DC power supply (1) output voltage range are 1kV to 2kV, and the power divider (6) is with input terminal, defeated
Outlet I and output end II, the potentiostat (17) have anode and cathode, the output end II of power divider (6) successively electric
Cable connects attenuator (7), transmission line I (8) and oscillograph (9), the sample cavity (12), bracket (11), semiconductor cooler
(15) it is sequentially connected from top to bottom with thermally conductive (16), bracket (11) is connected with thermometer (14), the optical tester (13)
Right above sample cavity (12), the optical tester (13) can launch laser and carry out spectrum point to the light of collection
Analysis, the laser include pump light and detection light；Sample cavity (12) includes cavity (12-1), plane mirror (12-2), working electrode
(12-3), to electrode (12-4), washer (12-5), sample (12-6), transmissive window (12-7), chamber lid (12-8), reference electrode
(12-9), connector I (12-10) and connector II (12-11), the plane mirror (12-2), working electrode (12-3), to electrode (12-
4), washer (12-5), sample (12-6) and transmissive window (12-7) are respectively positioned in cavity (12-1), the connector I of sample cavity (12)
(12-10) and connector II (12-11) are separately connected the anode and cathode of potentiostat (17), and potentiostat (17) is located at bracket
(11) below the sample cavity (12) in,
It is characterized in that: the output head anode of high-voltage DC power supply (1) successively cable connection charging resistor (2), charging cable (3), fire
The flowers are in blossom closes the defeated of the contact II (4-7) of (4), the rotary shaft (4-2) of spark switch (4), capacitor (5) and high-voltage DC power supply (1)
Outlet cathode；The spark switch (4) includes rotation motor (4-1), rotary shaft (4-2), horizon bar (4-3), trigger electrode I
(4-4), two contact I (4-5), trigger electrode II (4-6) and two contact II (4-7), rotary shaft (4-2) are vertically arranged to revolve
Turn on motor (4-1), be connected to rotary shaft (4-2) among horizon bar (4-3), horizon bar (4-3) length is 120 millimeters, triggering
Electrode I (4-4) and trigger electrode II (4-6) is the square that side length is 8 millimeters and is respectively arranged in horizon bar (4-3)
Both ends, the rotary shaft (4-2), horizon bar (4-3), trigger electrode I (4-4) and trigger electrode II (4-6) are electrically being connected；
Two contact I (4-5) are the identical metal cylinder of axis in the y-direction, and 10 millimeters and same are divided between two contact I (4-5)
Axis arrangement, the metal cylinder height is 10 millimeters, basal diameter is 10 millimeters, the axis and rotary shaft of contact I (4-5)
The axial line distance of (4-2) is 64 millimeters, and two contact II (4-7) are the metal strip of identical 1/6 circular shape, the circular arc
The center of circle be located on the axis of rotary shaft (4-2) and radius of curvature be 64 millimeters, two metal strips are at the direction y interval 10
Millimeter and in being arranged above and below, the electricity conducting mutually of two contact I (4-5), the electricity conducting mutually of two contact II (4-7), rotation
Motor (4-1) can make horizon bar (4-3) rotate in the horizontal plane by rotary shaft (4-2), and make trigger electrode I (4-
4) and trigger electrode II (4-6) can contactlessly pass through interval and two contact II (4-7) between two contact I (4-5)
Between interval；The cavity (12-1) is that the cylinder of axis in the y-direction is barrel-shaped, plane mirror (12-2) be axis in the y-direction
Cylindrical and be located at the bottom cavity (12-1), plane mirror (12-2) diameter is made by 30 millimeters and of polytetrafluoroethylene material, flat
The upper surface of face mirror (12-2) and side deposition are prepared with working electrode (12-3) and to electrode (12-4), working electrode (12-3)
With electrode (12-4) is made of gold and with a thickness of 500 microns；There are two through-hole, connector I (12- for the cavity side (12-1) tool
10) and connector II (12-11) can be respectively by two through-holes and working electrode (12-3) and to electrode (12-4) flat
The side of face mirror (12-2) is in close contact；Washer (12-5) is made and is located at the upper table of plane mirror (12-2) by epoxide resin material
Face, the outer diameter of washer (12-5) is 30 millimeters, internal diameter is 26 millimeters, thickness representative value is 5 to 30 microns, the position transmissive window (12-7)
In the top of washer (12-5), the diameter of transmissive window (12-7) is 30 millimeters, and sample (12-6) is placed in the internal diameter of washer (12-5)
Within, chamber lid (12-8) is installed on above cavity (12-1), and chamber lid (12-8) light transmission and can seal cavity (12-1),
Chamber lid (12-8) can will compress between transmissive window (12-7), washer (12-5) and plane mirror (12-2), chamber lid (12-8) and thoroughly
The via hole that window (12-7) all has the direction y is penetrated, reference electrode (12-9) can be inserted into sample (12-6) by the via hole, institute
State the touching of reference electrode (12-9) the successively rotary shaft (4-2), spark switch (4) of cable connection capacitor (5), spark switch (4)
Point I (4-5), the input terminal of power divider (6), the output end I of power divider (6), transmission line II (10) and connector II
(12-11)。
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| CN201811220426.2A CN109374535A (en) | 2018-10-10 | 2018-10-10 | A kind of electrochemical experimental device for spectral measurement |
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| CN110346408A (en) * | 2019-06-24 | 2019-10-18 | 金华职业技术学院 | A kind of method for testing heat of biological sample |
| CN110762207A (en) * | 2019-11-12 | 2020-02-07 | 国网重庆市电力公司电力科学研究院 | Sealing device for online electrochemical test of overhead ground wire and test method thereof |
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