CN110078042A - A kind of richness lithium LiFePO 4 material and its preparation method and application - Google Patents
A kind of richness lithium LiFePO 4 material and its preparation method and application Download PDFInfo
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- CN110078042A CN110078042A CN201910362503.6A CN201910362503A CN110078042A CN 110078042 A CN110078042 A CN 110078042A CN 201910362503 A CN201910362503 A CN 201910362503A CN 110078042 A CN110078042 A CN 110078042A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
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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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3277—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction being a redox reaction, e.g. detection by cyclic voltammetry
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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
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of rich lithium LiFePO 4 materials and its preparation method and application, belong to field of material technology.It using LiFePO4 as raw material during preparing the material, is assembled in button cell, then by the way that rich lithium LiFePO 4 material is made after carrying out charge and discharge cycles to button cell.The richness lithium LiFePO 4 material is having a size of micro-nano rank, and there is good lattice structure, it is coated on electrode and forms working electrode, for constructing NO electrochemica biological sensor, the sensor can be used for the direct growth of cell, it is capable of the NO molecule of the detection cell release of real-time in-situ, shows high sensitivity and selectivity in actually detected, and its stable electrochemical property, service life cycle are longer.The material preparation process is simple and convenient, the cost of raw material is cheap, is convenient for commercial applications.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of richness lithium LiFePO 4 material and preparation method thereof and answer
With.
Background technique
NO is a kind of cell messenger molecule, it is that L-arginine and oxygen are raw under the action of nitricoxide synthase (NOS)
At, it can spread in the cell rapidly or pass through cell membrane, complete the task of second messenger.It participates in adjusting thin under normal concentration
The vital movements such as metabolism, proliferation, differentiation, the apoptosis of born of the same parents, but then will lead to cytopathy when excessive concentration, cause abnormal
Cell death, so as to cause organism disease, wherein living with central nervous system, cardiovascular system, urogenital system, gastrointestinal tract
The relevant lesions such as dynamic, immunologic process are often not normal with increasing for NO concentration.Therefore, the NO of real-time detection cell release in situ
It is critically important for furtheing investigate its multiplicity effect in biosystem.
The method of NO detection is numerous, including fluorescence method, colorimetric method, electrochemical process, chromatography etc., and wherein electrochemical method has
Have the advantages that simple, sensitive, at low cost, detection is quick, therefore electrochemical sensor can be used, NO molecule is measured in real time.
However efficient NO Electrochemical Detection depends on the use of precious metal material more, and it is at high cost, it is unfavorable for generating use on a large scale.Cause
This, building has huge application prospect based on non-noble metal NO electrochemical sensor.
Summary of the invention
In view of this, one of the objects of the present invention is to provide a kind of preparation methods of rich lithium LiFePO 4 material；Purpose
Two be a kind of rich lithium LiFePO 4 material；The third purpose is to provide a kind of electrochemical sensor；The fourth purpose is to mention
For application of the electrochemical sensor in NO detection.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, a kind of preparation method of rich lithium LiFePO 4 material, described method includes following steps:
(1) LiFePO4, conductive black and Kynoar are added in N-Methyl pyrrolidone, must be mixed after mixing
The mixture is coated on aluminium foil and is dried, obtains the aluminium foil of load LiFePO4 by object, with the load LiFePO4
Aluminium foil is anode, and metal lithium sheet is to electrode, and polyethene microporous membrane is diaphragm, and hexafluoro phosphorus lithium electrolyte is electrolyte, after assembling
Obtain button cell；
(2) charge and discharge cycles are carried out to the button cell obtained in step (1), then dismantles the button cell and takes out
Anode, the anode is cleaned, drying after scrape it is described anode on rich lithium LiFePO 4 material.
Preferably, in step (1), the mass ratio of the LiFePO4, conductive black and Kynoar is 4-9:
0.5-3:0.5-3；The aluminium foil with a thickness of 160-180 μm, in the hexafluoro phosphorus lithium electrolyte concentration of hexafluoro phosphorus lithium be 1M,
The button cell is CR250 type button cell.
Preferably, in step (1), the drying is specially the dry 10-12h at 110-120 DEG C.
Preferably, in step (2), the charge and discharge cycles be specially voltage range be 2.0 ± 0.2V to 4.2 ±
0.3V, electric current 0.1-0.5C, temperature is first discharged under conditions of being 23-27 DEG C to charge afterwards, to discharge into minimum voltage after circulation
For end-state.
Preferably, in step (2), using organic solution as cleaning solution when the cleaning, the drying is specially at 20-80 DEG C
Lower dry 2-5h.
2, the rich lithium LiFePO 4 material prepared by the method.
3, a kind of electrochemical sensor, including electrochemical workstation, working electrode, to electrode, reference electrode, electrolytic cell and
Electrolyte, the working electrode surface are coated with the rich lithium LiFePO 4 material.
Preferably, the working electrode is prepared as follows:
Rich lithium LiFePO 4 material is dispersed in water with the matched proportion density of 2.8-3.8mg/mL, it is molten to obtain electrode modification
The electrode modification solution is coated on electrode by liquid, dry.
Preferably, the drying is specially the dry 20-60min at 20-100 DEG C.
4, application of a kind of electrochemical sensor in NO detection.
The beneficial effects of the present invention are: the present invention provides a kind of rich lithium LiFePO 4 material and preparation method thereof and answer
With the richness lithium LiFePO 4 material has good lattice structure having a size of micro-nano rank, is coated onto shape on electrode
At working electrode, for constructing NO electrochemica biological sensor, which can be used for the direct growth of cell, can be real-time
The NO molecule of detection cell release in situ shows high sensitivity and selectivity, and its electrochemistry in actually detected
Performance is stable, service life cycle is longer.The material preparation process is simple and convenient, the cost of raw material is cheap, answers convenient for commercialization
With.
Other advantages, target and feature of the invention will be illustrated in the following description to a certain extent, and
And to a certain extent, based on will be apparent to those skilled in the art to investigating hereafter, Huo Zheke
To be instructed from the practice of the present invention.Target of the invention and other advantages can be realized by following specification and
It obtains.
Detailed description of the invention
To make the objectives, technical solutions, and advantages of the present invention clearer, the present invention is made below in conjunction with attached drawing excellent
The detailed description of choosing, in which:
Fig. 1 is the scanning electron microscope (SEM) photograph and perspective electron microscope of the rich lithium LiFePO 4 material prepared in embodiment 1；(a in Fig. 1
For scanning electron microscope (SEM) photograph, b is transmission electron microscope picture in Fig. 1)
Fig. 2 is the X-ray diffractogram of the rich lithium LiFePO 4 material prepared in embodiment 1；
Fig. 3 is the scanning electron microscope (SEM) photograph and perspective electron microscope of the rich lithium LiFePO 4 material prepared in embodiment 2；(a in Fig. 3
For scanning electron microscope (SEM) photograph, b is transmission electron microscope picture in Fig. 3)
Fig. 4 is the X-ray diffractogram of the rich lithium LiFePO 4 material prepared in embodiment 2；
Fig. 5 is the scanning electron microscope (SEM) photograph and perspective electron microscope of the rich lithium LiFePO 4 material prepared in embodiment 3；(a in Fig. 5
For scanning electron microscope (SEM) photograph, b is transmission electron microscope picture in Fig. 5)
Fig. 6 is the X-ray diffractogram of the rich lithium LiFePO 4 material prepared in embodiment 3；
Fig. 7 is the lithium ion content test result figure of the LiFePO 4 material discharged under different voltages in embodiment 1；
Fig. 8 is in the case where voltage range is -0.2-1.1V, and the sensor constructed in embodiment 1 responds the cyclic voltammetric of NO
Test result figure；
Fig. 9 is the chrono-amperometric response test result to NO that the sensor constructed in embodiment 1 is measured at 0.85V
Figure；
Figure 10 is the graph of relation obtained between NO concentration and current-responsive by Fig. 9；
Figure 11 be in embodiment 1 sensor that constructs to disturbance ingredient selectivity test result figure；
Figure 12 is the sensor stability test result figure constructed in embodiment 1；
Figure 13 is that the sensor constructed in embodiment 1 carries out the cell in direct long cell and culture dish on the electrode
The current-responsive test result figure of NO detection.
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Embodiment 1
It prepares rich lithium LiFePO 4 material and coats the working electrode of the material, and construct nitric oxide electrochemical sensor
It (1) is 8:1:1 by LiFePO4, conductive charcoal by the mass ratio of LiFePO4, conductive black and Kynoar
Black and Kynoar is added in N-Methyl pyrrolidone, and mixture is obtained after mixing, which is coated in a thickness of 170 μm
Aluminium foil on and the dry 12h at 120 DEG C, obtain the aluminium foil of load LiFePO4, be positive with the aluminium foil of the load LiFePO4
Pole, metal lithium sheet are to electrode, and polyethene microporous membrane is diaphragm, and the hexafluoro phosphorus lithium electrolyte that the concentration of hexafluoro phosphorus lithium is 1M is electricity
Liquid is solved, is assembled into CR250 type button cell in the glove box full of argon gas；
(2) charge and discharge cycles are carried out to the CR250 type button cell obtained in step (1), is specially in voltage range
1.8-4.2V, electric current 0.3C, temperature is first discharged under conditions of being 25 DEG C to charge afterwards, discharges into 1.8V after 3 charge and discharge cycles
For end-state, then dismantles the CR250 type button cell and take out anode, by anode through washes of absolute alcohol, at 60 DEG C
The rich lithium LiFePO 4 material on anode is scraped after dry 4h；
(3) deionization is dispersed with the matched proportion density of 3.3mg/mL by the rich lithium LiFePO 4 material prepared in step (2)
In water, electrode modification solution is obtained, the electrode modification solution is added drop-wise to area as 0.07cm by 5 μ L2Screen printing electrode on,
Dry 30min, is made the working electrode for being coated with rich lithium LiFePO 4 material at 50 DEG C；
(4) surface obtained in step (3) is coated with to the working electrode and electrochemical operation of pyrophosphoric acid cobalt nano material
It stands, to electrode (screen printing carbon electrode), reference electrode (screen printing carbon electrode), electrolytic cell and electrolyte, (concentration is
The phosphate buffer solution of 0.01mol/L, pH=7.4) it is assembled into nitric oxide electrochemical sensor together.
Embodiment 2
It prepares rich lithium LiFePO 4 material and coats the working electrode of the material, and construct nitric oxide electrochemical sensor
It (1) is 4:3:3 by LiFePO4, conductive charcoal by the mass ratio of LiFePO4, conductive black and Kynoar
Black and Kynoar is added in N-Methyl pyrrolidone, and mixture is obtained after mixing, which is coated in a thickness of 180 μm
Aluminium foil on and the dry 10h at 115 DEG C, obtain the aluminium foil of load LiFePO4, be positive with the aluminium foil of the load LiFePO4
Pole, metal lithium sheet are to electrode, and polyethene microporous membrane is diaphragm, and the hexafluoro phosphorus lithium electrolyte that the concentration of hexafluoro phosphorus lithium is 1M is electricity
Liquid is solved, is assembled into CR250 type button cell in the glove box full of argon gas；
(2) charge and discharge cycles are carried out to the CR250 type button cell obtained in step (1), is specially in voltage range
2.0-3.9V, electric current 0.1C, temperature is first discharged under conditions of being 23 DEG C to charge afterwards, discharges into 2.0V after 3 charge and discharge cycles
For end-state, then dismantles the CR250 type button cell and take out anode, by anode through washes of absolute alcohol, at 20 DEG C
The rich lithium LiFePO 4 material on anode is scraped after dry 5h；
(3) deionization is dispersed with the matched proportion density of 3.8mg/mL by the rich lithium LiFePO 4 material prepared in step (2)
In water, electrode modification solution is obtained, the electrode modification solution is added drop-wise to area as 0.07cm by 5 μ L2Screen printing electrode on,
Dry 60min, is made the working electrode for being coated with rich lithium LiFePO 4 material at 20 DEG C；
(4) surface obtained in step (3) is coated with to the working electrode and electrochemical operation of pyrophosphoric acid cobalt nano material
It stands, to electrode (screen printing carbon electrode), reference electrode (silk-screen printing Ag/AgCl electrode), electrolytic cell and electrolyte, (concentration is
The phosphate buffer solution of 0.1mol/L, pH=7.2) it is assembled into nitric oxide electrochemical sensor together.
Embodiment 3
It prepares rich lithium LiFePO 4 material and coats the working electrode of the material, and construct nitric oxide electrochemical sensor
(1) by LiFePO4, conductive black and Kynoar mass ratio be 9:0.5:0.5 by LiFePO4, lead
Electric carbon black and Kynoar are added in N-Methyl pyrrolidone, after mixing mixture, by the mixture be coated in a thickness of
11h is dried on 160 μm of aluminium foil and at 110 DEG C, the aluminium foil of load LiFePO4 is obtained, with the aluminium foil of the load LiFePO4
For anode, metal lithium sheet is to electrode, and polyethene microporous membrane is diaphragm, and the concentration of hexafluoro phosphorus lithium is the hexafluoro phosphorus lithium electrolyte of 1M
For electrolyte, CR250 type button cell is assembled into the glove box full of argon gas；
(2) charge and discharge cycles are carried out to the CR250 type button cell obtained in step (1), is specially in voltage range
2.2-4.5V, electric current 0.5C, temperature is first discharged under conditions of being 27 DEG C to charge afterwards, discharges into 2.2V after 3 charge and discharge cycles
For end-state, then dismantles the CR250 type button cell and take out anode, by anode through washes of absolute alcohol, at 80 DEG C
The rich lithium LiFePO 4 material on anode is scraped after dry 2h；
(3) deionization is dispersed with the matched proportion density of 2.8mg/mL by the rich lithium LiFePO 4 material prepared in step (2)
In water, electrode modification solution is obtained, the electrode modification solution is added drop-wise to area as 0.1cm by 10 μ L2Screen printing electrode on,
Dry 20min, is made the working electrode for being coated with rich lithium LiFePO 4 material at 100 DEG C；
(4) surface obtained in step (3) is coated with to the working electrode and electrochemical operation of pyrophosphoric acid cobalt nano material
It stands, to electrode (screen printing carbon electrode), electrolytic cell and the electrolyte (phosphate-buffered of concentration 0.05mol/L, pH=7.0
Solution) it is assembled into nitric oxide electrochemical sensor together.
Fig. 1 is the scanning electron microscope (SEM) photograph and perspective electron microscope of the rich lithium LiFePO 4 material prepared in embodiment 1, wherein Fig. 1
Middle a is scanning electron microscope (SEM) photograph, and b is transmission electron microscope picture in Fig. 1, and as shown in Figure 1, which is micro/nano level
Not, and there is good lattice structure.
Fig. 2 is the X-ray diffractogram of the rich lithium LiFePO 4 material prepared in embodiment 1, as shown in Figure 2, the richness lithium phosphorus
Sour iron lithium has preferable LiFePO 4 material lattice structure.
Fig. 3 is the scanning electron microscope (SEM) photograph and perspective electron microscope of the rich lithium LiFePO 4 material prepared in embodiment 2, wherein Fig. 3
Middle a is scanning electron microscope (SEM) photograph, and b is transmission electron microscope picture in Fig. 3, from the figure 3, it may be seen that the richness lithium LiFePO 4 material size is micro/nano level
Not, and there is good lattice structure.
Fig. 4 is the X-ray diffractogram of the rich lithium LiFePO 4 material prepared in embodiment 2, as shown in Figure 4, the richness lithium phosphorus
Sour iron lithium has preferable LiFePO 4 material lattice structure.
Fig. 5 is the scanning electron microscope (SEM) photograph and perspective electron microscope of the rich lithium LiFePO 4 material prepared in embodiment 3, wherein Fig. 5
Middle a is scanning electron microscope (SEM) photograph, and b is transmission electron microscope picture in Fig. 5, and as shown in Figure 5, which is micro/nano level
Not, and there is good lattice structure.
Fig. 6 is the X-ray diffractogram of the rich lithium LiFePO 4 material prepared in embodiment 3, it will be appreciated from fig. 6 that the richness lithium phosphorus
Sour iron lithium has preferable LiFePO 4 material lattice structure.
Embodiment 4
The LiFePO 4 material under different voltages is discharged into Example 1, is surveyed using Inductively coupled plasma-mass spectrometry
The lithium ion content of different LiFePO 4 materials is obtained, and the lithium ion content of different LiFePO 4 materials is compared, as a result
As shown in fig. 7, as shown in Figure 7, the lithium ion content in LiFePO 4 material when discharging into minimum voltage is higher than theoretical value
(4.4%, w/w), it was demonstrated that the material is rich lithium LiFePO 4 material.
Embodiment 5
A certain amount of NO solution is added in the electrolyte of the sensor constructed in embodiment 1, voltage range be-
The sensor is tested under 0.2-1.1V to respond the cyclic voltammetric of NO, while being lied prostrate with circulation of the sensor to phosphate buffer solution
Peace response is used as blank control.As a result as shown in figure 8, as shown in Figure 8, the sensor constructed in embodiment 1 appearance in 0.85V
The oxidation peak of NO, illustrates that the sensor has apparent electrochemical catalytic oxidation ability to NO.
Embodiment 6
Timing of the sensor constructed in testing example 1 under the crest voltage (0.85V) of cyclic voltammetry curve to NO
The NO solution of various concentration, time are added in the electrolyte for the sensor that when test continuously constructs into embodiment 1 for current-responsive
Between be divided into 50s, the relation curve of recording responses time and current value to get the sensor to the peace times response diagram of NO, as a result such as
Shown in Fig. 9, the small figure in the upper right corner is that the NO of various concentration is added as shown in Figure 9 in influence time figure of the sensor to NO in figure
Afterwards, sensor current response is continuously increased and reaches within the faster time stable state, and the response time is less than 2s；It is obtained by Fig. 9
The graph of relation between NO concentration and current-responsive is obtained, as shown in Figure 10, as shown in Figure 10, the current-responsive of the sensor exists
NO concentration is 5 × 10-10-2.9×10-7Good linear relationship is presented within the scope of mol/L, detection is limited to 1.2 × 10-10mol/
L。
Embodiment 7
In the electrolyte for the sensor that the solution of different material is added sequentially to construct in embodiment 1, the sensing is tested
Device responds the chrono-amperometric of disturbance composition, test voltage 0.85V, and the time interval that disturbance object is added is 50s,
The sensor is obtained to the ampere response curve of disturbance ingredient selectivity test, as a result as shown in figure 11, as shown in Figure 11,
The sensor has good selectivity NO.
Embodiment 8
NO solution is added in the electrolytic cell of the sensor constructed in embodiment 1, is surveyed in the case where voltage range is -0.2-1.1V
Examination placed the sensor of different number of days and respond to the cyclic voltammetric of NO, and when test uses the same electrochemical sensor, and every 5
Its test is primary, and the concentration for the NO being added every time remains unchanged, and tests 7 times altogether to get the stability test knot in storage 30 days
Fruit figure, as a result as shown in figure 12, as shown in Figure 12, which has good measuring stability.
Embodiment 9
By the cell inoculation obtained working electrode surface for being coated with rich lithium LiFePO 4 material in embodiment 1, and
Cell obtains the electrode that cell in-situ is grown, the sensor which is constructed in embodiment 1 after training sample case culture 12h
In, and the chrono-amperometric response of the cell release NO under acetylcholine medicine irritation is tested, the sensor is obtained to electrode growth
The NO of cell release carries out the current-responsive of in situ detection.In comparative experiments, by the electrolysis of the sensor constructed in embodiment 1
Pond replaces with the culture dish that growth has cell, and it is 0.01mol/L that electrolyte, which is still concentration, and the phosphate-buffered of pH=7.4 is molten
Liquid tests the chrono-amperometric response of the cell release NO under acetylcholine medicine irritation, obtains the cell release NO in culture dish
Current-responsive.As a result as shown in figure 13, as shown in Figure 13, it is grown directly upon the cell in the sensor on working electrode and releases institute
The NO put can be by more efficient detection.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of the technical program, should all be covered in the present invention
Scope of the claims in.
Claims (10)
1. a kind of preparation method of richness lithium LiFePO 4 material, which is characterized in that described method includes following steps:
(1) LiFePO4, conductive black and Kynoar are added in N-Methyl pyrrolidone, mixture is obtained after mixing, it will
The mixture is coated on aluminium foil and dries, and obtains the aluminium foil of load LiFePO4, with the aluminium foil of the load LiFePO4
For anode, metal lithium sheet is to electrode, and polyethene microporous membrane is diaphragm, and hexafluoro phosphorus lithium electrolyte is electrolyte, is obtained after assembling
Button cell；
(2) charge and discharge cycles are carried out to the button cell obtained in step (1), then dismantle the button cell and taken out just
Pole, the anode is cleaned, drying after scrape it is described anode on rich lithium LiFePO 4 material.
2. the method as described in claim 1, which is characterized in that in step (1), the LiFePO4, conductive black and poly- inclined
The mass ratio of vinyl fluoride is 4-9:0.5-3:0.5-3；The aluminium foil with a thickness of 160-180 μm, hexafluoro phosphorus lithium electrolysis
The concentration of hexafluoro phosphorus lithium is 1M in liquid, and the button cell is CR250 type button cell.
3. the method as described in claim 1, which is characterized in that in step (1), the drying is specially at 110-120 DEG C
Dry 10-12h.
4. the method as described in claim 1, which is characterized in that in step (2), the charge and discharge cycles are specially in voltage model
It encloses for 2.0 ± 0.2V to 4.2 ± 0.3V, electric current 0.1-0.5C, temperature is first discharged under conditions of being 23-27 DEG C to charge afterwards, with
It is end-state that minimum voltage is discharged into after circulation.
5. the method as described in claim 1, which is characterized in that with organic solution be cleaning when the cleaning in step (2)
Liquid, the drying are specially the dry 2-5h at 20-80 DEG C.
6. by the rich lithium LiFePO 4 material of the described in any item method preparations of claim 1-5.
7. a kind of electrochemical sensor, including electrochemical workstation, working electrode, to electrode, reference electrode, electrolytic cell and electrolysis
Liquid, which is characterized in that the working electrode surface is coated with rich lithium LiFePO 4 material as claimed in claim 6.
8. a kind of electrochemical sensor as claimed in claim 7, which is characterized in that the working electrode is made as follows
It is standby:
Rich lithium LiFePO 4 material is dispersed in water with the matched proportion density of 2.8-3.8mg/mL, obtains electrode modification solution, it will
The electrode modification solution is coated on electrode, dry.
9. a kind of electrochemical sensor as claimed in claim 8, which is characterized in that the drying is specially at 20-100 DEG C
Dry 20-60min.
10. a kind of application of the electrochemical sensor as claimed in claim 7 in NO detection.
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| CN112285183A (en) * | 2020-10-10 | 2021-01-29 | 广州大学 | Membrane-free all-solid-state ion selective electrode and preparation method and application thereof |
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