CN108918329A - The portable measuring method for measuring of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode - Google Patents
The portable measuring method for measuring of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode Download PDFInfo
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- CN108918329A CN108918329A CN201810359162.2A CN201810359162A CN108918329A CN 108918329 A CN108918329 A CN 108918329A CN 201810359162 A CN201810359162 A CN 201810359162A CN 108918329 A CN108918329 A CN 108918329A
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- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The invention discloses a kind of portable measuring method for measuring of phosphorus content in carbon coating vanadium phosphate sodium positive electrode, belong to electrochemical analysis techniques field.The portable measuring method for measuring of phosphorus content, operating process be in a kind of carbon coating vanadium phosphate sodium positive electrode of the invention：A certain amount of carbon coating vanadium phosphate sodium is weighed, it is calcined in air, the mass change of record calcining front and back, then by the object phase component of product after analysis calcining, the phosphorus content of carbon coating vanadium phosphate sodium can be extrapolated.This method can not only accurately measure the content of carbon in carbon coating vanadium phosphate sodium, and simple process compared with other measurement methods, and cost is relatively low, without expensive detection device, can carry out in the experimental situation of general condition.
Description
Technical field
The present invention relates to a kind of portable measuring method for measuring of carbon content in carbon coating vanadium phosphate sodium positive electrode, belong to sodium ion
Cell positive material technical field.
Background technique
Recently, sodium-ion battery due to sodium it is resourceful, cheap, in electrochemistry secondary power supply technology take off grain husk and
Out.Particularly, with the vanadium phosphate sodium Na of NASICON structure3V2(PO4)3(NVP) positive electrode is because brilliant with stable three-dimensional
Body frame structure and higher working voltage platform and become sodium-ion battery research hot topic.But the electronics of NVP is electric
Conductance is lower, and chemical property is not satisfactory, especially under larger current density.Currently, most universal, easy Improving Measurements
It is that carbon coating (NVP/C) is carried out to NVP, i.e., organism is introduced in sample preparation procedure, then in an inert atmosphere in high temperature
Amorphous carbon is translated by pyrolytic process down and is coated on the surface of NVP, so that the electron conductivity of NVP is improved, into
And improve its chemical property.
The control of carbon content is very important in above-mentioned carbon coating vanadium phosphate sodium, very few that raising electronic conductivity is not achieved
Effect, excessively can then reduce the capacity (carbon does not have capacity contribution in positive electrode) and tap density of entire electrode.Therefore,
Carbon content in accurate measurement and control carbon coating vanadium phosphate sodium is for guaranteeing that the service performance of NVP just has great importance.
Currently, the measurement of phosphorus content mainly has elemental microanalysis method and thermogravimetry in NVP/C.Elemental microanalysis method is to rely on
Elemental analyser is measured, and principle is that sample is carried out oxidizing fire at high temperature, makes carbon conversion CO2Gas, then
Into separation detection unit (gas chromatographic column+thermal conductivity detector (TCD)), achieve the purpose that quantitative analysis.For example, Klee etc.
(Journal of Power Sources 2016,313:73-80) utilize EuroVector elemental analyser and Lim etc.
(Journal of Materials Chemistry A 2014,2(46):19569-19922) utilize Elementar element point
Analyzer is determined the phosphorus content in NVP/C.Although this method measurement result is accurate, elemental analyser is costly
(general 500,000 or more).Thermogravimetry is using thermogravimetric analyzer (mainly by precision balance, stove, temperature programmed control system, note
Recording system etc.) measurement of species quality variation with temperature relationship.By analyzing thermogravimetric curve, NVP/ is extrapolated according to weight loss
Phosphorus content (Nano Energy 2016,20 in C:11-19；Electrochimica Acta,2015,155:23-28).This
Expensive thermogravimetric analyzer (general 300,000 yuan or more) is not only needed, but also its measurement result there may be certain deviation
(it there may be V during weightless3+Oxidation weight gain).
Therefore, a kind of portable measuring method for measuring of carbon content in carbon coating vanadium phosphate sodium positive electrode is developed, and guarantees it
Measurement accuracy has great importance for the carbon content control of carbon coating vanadium phosphate sodium and its guarantee of performance.
Summary of the invention
1. technical problems to be solved by the inivention
It is an object of the invention to overcome in existing carbon coating vanadium phosphate sodium Determination of Carbon there are expensive equipment, at
The deficiency for the problems such as this is high, and provide the portable measuring method for measuring of phosphorus content in carbon coating vanadium phosphate sodium positive electrode.Using this
The method of invention can accurately measure the carbon content in carbon coating vanadium phosphate sodium, and measuring method is simple, easy to operate, convenient for pushing away
Wide application.
2. technical solution
In order to achieve the above objectives, technical solution provided by the invention is：
The portable measuring method for measuring of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode of the invention, by a certain amount of carbon
Vanadium phosphate sodium is coated, is placed in air and is calcined, the mass change of record calcining front and back, in conjunction with the object of calcining front and back product
Phase component analysis, can determine the phosphorus content in carbon coating vanadium phosphate sodium.
Further, measuring method of the invention specifically includes following steps：
(1) first sample to be tested is dried；
(2) the carbon coating vanadium phosphate sodium after a certain amount of drying is weighed, quality is denoted as M1；
(3) the carbon coating vanadium phosphate sodium after weighed drying is placed in Muffle furnace at 490-510 DEG C and carries out calcining 10-
13 hours；
(4) after calcining, it is down to room temperature to Muffle furnace, takes out product, weighing, quality is denoted as M2；
(5) it according to the chemical formula of carbon coating vanadium phosphate sodium calcination reaction, that is, calculates and obtains the carbon in carbon coating vanadium phosphate sodium
Content (xwt%).
Further, after carbon coating vanadium phosphate sodium being placed in Muffle furnace in step (3), control heating rate 1-3 DEG C/
Minute.
Further, control calcination temperature is 500 DEG C, calcination time 12h.
Further, calcined product is subjected to X-ray diffraction test, analyzes its object phase composition, obtains carbon coating phosphoric acid
Vanadium sodium calcining chemical equation be：
Further, the carbon content (x wt%) in the carbon coating vanadium phosphate sodium can be calculated by following equation：
Further, that sample to be tested is placed in air dry oven at 80-100 DEG C dry 8-24 in step (1) is small
When.
3. beneficial effect
Using technical solution provided by the invention, compared with prior art, there is following remarkable result：
(1) in a kind of carbon coating vanadium phosphate sodium positive electrode of the invention phosphorus content portable measuring method for measuring, by by carbon
Cladding vanadium phosphate sodium, which is placed in air, to be calcined, the mass change of record reaction front and back, then by product after calcining
Object phase component is analyzed, and the phosphorus content in carbon coating vanadium phosphate sodium positive electrode can be extrapolated, with existing other methods phase
Than measuring method of the invention is easy to operate, and cost is relatively low, and without expensive detection device, and its measurement result is more accurate.
(2) in a kind of carbon coating vanadium phosphate sodium positive electrode of the invention phosphorus content portable measuring method for measuring, penetrated by X-
The object phase component of products therefrom after calcining is analyzed in the test of line diffraction, so as to accurately show that carbon coating vanadium phosphate sodium passes through
The type of products therefrom and its chemical equation for carrying out calcination reaction after calcination reaction, thus in carbon coating vanadium phosphate sodium
The Accurate Determining of carbon content has established necessary basis.
(3) in a kind of carbon coating vanadium phosphate sodium positive electrode of the invention phosphorus content portable measuring method for measuring, carbon coating phosphorus
The calcine technology of sour vanadium sodium, especially calcination temperature, calcination time and heating rate for measurement result accuracy to close weight
It wants, the present invention is by carrying out strict control to calcine technology parameter, so that carbon coating vanadium phosphate on the one hand can both be effectively ensured
Fully calcined, another aspect and the melting that mixed phase in calcination process can be effectively prevent of sodium, and then influence the measurement of quality.
Detailed description of the invention
Fig. 1 is the X-ray diffracting spectrum of gained calcined product in step of the present invention (3).
Specific embodiment
The portable measuring method for measuring of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode of the invention, by a certain amount of carbon
Vanadium phosphate sodium is coated, is placed in air and is calcined, the mass change of record calcining front and back, in conjunction with the object of calcining front and back product
Phase component analysis, can determine the phosphorus content in carbon coating vanadium phosphate sodium, specifically include following steps：
(1) first sample to be tested is placed in air dry oven at 80-100 DEG C 8-24 hours dry；
(2) the carbon coating vanadium phosphate sodium after a certain amount of drying is weighed, quality is denoted as M1；
(3) the carbon coating vanadium phosphate sodium after weighed drying is placed in Muffle furnace at 490-510 DEG C and carries out calcining 10-
13 hours, heating rate was controlled at 1-3 DEG C/min, it is furthermore preferred that control calcination temperature is 500 DEG C, calcination time 12h；
(4) after calcining, it is down to room temperature to Muffle furnace, takes out product, weighing, quality is denoted as M2；
(5) calcined product is subjected to X-ray diffraction test, analyzes its object phase composition, show that carbon coating vanadium phosphate sodium is calcined
Chemical equation be：Knot
The mass change for closing the chemical formula and reaction front and back, that is, calculate and obtain the carbon content (x wt%) in carbon coating vanadium phosphate sodium：
Carbon coating is a kind of common modification means of vanadium phosphate sodium positive electrode, and being coated processing can be effectively improved
The chemical property of vanadium phosphate sodium positive electrode, wherein the covering amount of carbon is most important for covered effect.But in the prior art
The measurement that carbon content is coated in carbon coating vanadium phosphate sodium usually requires to carry out by certain external equipment, external equipment valence used
Lattice are expensive, are unsuitable for promoting and applying.Based on problem above, the present invention is had investigated in a kind of carbon coating vanadium phosphate sodium positive electrode
Carbon coating vanadium phosphate sodium is placed in air and calcines by the portable measuring method for measuring of phosphorus content, in conjunction with the quality of calcining front and back
Variation and carbon coating vanadium phosphate sodium carry out the chemical formula of calcination reaction, can extrapolate carbon containing in carbon coating vanadium phosphate sodium
Amount.Wherein, it should be noted that inferred according to common sense, vanadium should be able to be changed into 5 valences, art technology from trivalent after heat treatment
Personnel, which not will recognize that, is measured analysis to calcined product object phase composition again, but applicant is through X-ray diffraction test analysis
It was found that the vanadium in the present invention after calcining in carbon coating vanadium phosphate sodium is but changed into 4 valences, and combine X-ray diffraction test analysis
Result be inferred to calcined product of the invention be Na2(VP2O8) and a small amount of V4O9Miscellaneous phase (as shown in Figure 1), concludes therefrom that
Correct carbon coating vanadium phosphate sodium calcination reaction equation, so that base has been established in the measurement for carbon content in carbon coating vanadium phosphate sodium
Plinth.
It should be noted the control of calcine technology in the present invention, especially calcination temperature and time and heating speed
The control of rate is most important for the accuracy for guaranteeing determination of carbon content result.The present invention is tight by carrying out to calcine technology parameter
Lattice control, so that the full combustion of amorphous carbon in carbon coating vanadium phosphate sodium on the one hand can be both effectively ensured, on the other hand again
Can effectively prevent in calcination process because calcination temperature it is excessively high caused by mixed phase melting, and then influence quality measurement.In addition,
For the type of calcined product, there is also certain influences for the control of calcine technology parameter, when calcination temperature changes, meeting
The variation for causing calcined product, leads to the presence of different price vanadium, to influence the accurate of carbon content in carbon coating vanadium phosphate sodium
Measurement.Wherein, when calcination temperature is 500 DEG C, and calcination time is 12h, measurement result is the most accurate.
To further appreciate that the contents of the present invention, the present invention is described in detail combined with specific embodiments below.
Embodiment 1
Sample to be tested is 24 hours dry at 80 DEG C in air dry oven, after cooling, precise M1=5.000g is waited for
Sample is put into ready crucible.Then the crucible for containing sample is put into Muffle furnace, calcines 12 at 500 DEG C in air
Hour (heating rate is 1 DEG C/min).After calcining, it is down to room temperature to Muffle furnace, takes out product, correct amount is denoted as M2
=4.575g.According to the reaction equation that carbon coating vanadium phosphate sodium is calcined in air, the carbon content in carbon coating vanadium phosphate sodium is calculated
(x wt%), calculates according to following formula：
In the implementation case, the weight M of sample to be tested1=5.000g；The weight M of sample to be tested after calcining2=4.575g；
The carbon content x wt%=11.97% of required carbon coating vanadium phosphate sodium.
Embodiment 2
Sample to be tested is 8 hours dry at 100 DEG C in air dry oven, after cooling, precise M1=6.000g is waited for
Sample is put into ready crucible.Then the crucible for containing sample is put into Muffle furnace, calcines 12 at 500 DEG C in air
Hour (heating rate is 3 DEG C/min).After calcining, it is down to room temperature to Muffle furnace, takes out product, correct amount is denoted as M2
=5.820g.According to the reaction equation that carbon coating vanadium phosphate sodium is calcined in air, the carbon content in carbon coating vanadium phosphate sodium is calculated
(xwt%), it is calculated according to following formula：
In the implementation case, the weight M of sample to be tested1=6.000g；The weight M of sample to be tested after calcining2=5.820g；
The carbon content x wt%=6.68% of required carbon coating vanadium phosphate sodium.
Embodiment 3
Sample to be tested is 12 hours dry at 90 DEG C in air dry oven, after cooling, precise M1=10.000g is waited for
Sample is put into ready crucible.Then the crucible for containing sample is put into Muffle furnace, calcines 12 at 500 DEG C in air
Hour (heating rate is 2 DEG C/min).After calcining, it is down to room temperature to Muffle furnace, takes out product, correct amount is denoted as M2
=9.605g.According to the reaction equation that carbon coating vanadium phosphate sodium is calcined in air, the carbon content in carbon coating vanadium phosphate sodium is calculated
(xwt%), it is calculated according to following formula：
In the implementation case, the weight M of sample to be tested1=10.000g；The weight M of sample to be tested after calcining2=9.605g；
The carbon content x wt%=7.59% of required carbon coating vanadium phosphate sodium.
Claims (7)
1. the portable measuring method for measuring of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode, it is characterised in that：It will be a certain amount of
Carbon coating vanadium phosphate sodium, is placed in air and is calcined, the mass change of record calcining front and back, in conjunction with the object of product after calcining
Phase component analysis, can determine the phosphorus content in carbon coating vanadium phosphate sodium.
2. the portable measuring method for measuring of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode according to claim 1,
It is characterized in that, specifically includes following steps：
(1) first sample to be tested is dried；
(2) the carbon coating vanadium phosphate sodium after a certain amount of drying is weighed, quality is denoted as M1；
(3) the carbon coating vanadium phosphate sodium after weighed drying is placed in Muffle furnace carried out at 490-510 DEG C calcining 10-13 it is small
When；
(4) after calcining, it is down to room temperature to Muffle furnace, takes out product, weighing, quality is denoted as M2；
(5) it according to the chemical formula of carbon coating vanadium phosphate sodium calcination reaction, that is, calculates and obtains the carbon content in carbon coating vanadium phosphate sodium
(xwt%).
3. the portable measuring method for measuring of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode according to claim 2,
It is characterized in that：After carbon coating vanadium phosphate sodium is placed in Muffle furnace in step (3), heating rate is controlled at 1-3 DEG C/min.
4. the portable measuring method for measuring of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode according to claim 2,
It is characterized in that：Controlling calcination temperature is 500 DEG C, calcination time 12h.
5. the portable measuring method for measuring of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode according to claim 4,
It is characterized in that：Calcined product is subjected to X-ray diffraction test, analyzes its object phase composition, extrapolates the calcining of carbon coating vanadium phosphate sodium
Chemical equation be：
6. the simple survey of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode according to any one of claim 2-5
Determine method, it is characterised in that：Carbon content (x wt%) in the carbon coating vanadium phosphate sodium can be calculated by following equation：
7. the simple survey of phosphorus content in a kind of carbon coating vanadium phosphate sodium positive electrode according to any one of claim 2-5
Determine method, it is characterised in that：It is small that sample to be tested is placed in air dry oven at 80-100 DEG C dry 8-24 in step (1)
When.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61191950A (en) * | 1985-02-21 | 1986-08-26 | Mitsubishi Heavy Ind Ltd | Industrial analysis for coal and coke |
| CN102569797A (en) * | 2012-01-20 | 2012-07-11 | 中国科学院宁波材料技术与工程研究所 | Novel phosphate based composite cathode material, its preparation method and application thereof |
| CN102854085A (en) * | 2012-09-17 | 2013-01-02 | 徐剑晖 | Method for measuring carbon content in lithium iron phosphate |
| CN107611367A (en) * | 2017-08-04 | 2018-01-19 | 中南大学 | A kind of porous spherical carbon coating vanadium phosphate sodium composite positive pole and preparation method thereof |
-
2018
- 2018-04-20 CN CN201810359162.2A patent/CN108918329A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61191950A (en) * | 1985-02-21 | 1986-08-26 | Mitsubishi Heavy Ind Ltd | Industrial analysis for coal and coke |
| CN102569797A (en) * | 2012-01-20 | 2012-07-11 | 中国科学院宁波材料技术与工程研究所 | Novel phosphate based composite cathode material, its preparation method and application thereof |
| CN102854085A (en) * | 2012-09-17 | 2013-01-02 | 徐剑晖 | Method for measuring carbon content in lithium iron phosphate |
| CN107611367A (en) * | 2017-08-04 | 2018-01-19 | 中南大学 | A kind of porous spherical carbon coating vanadium phosphate sodium composite positive pole and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 张香华 等: "溶胶-凝胶法制备钠离子电池正极材料Na3V2(PO4)3", 《第三届钒钛微合金化高强钢开发应用技术暨第四届钒产业先进技术交流会论文集》 * |
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