CN110333194A - A kind of method of quantitative analysis carbon nano electronic transfer ability - Google Patents

A kind of method of quantitative analysis carbon nano electronic transfer ability Download PDF

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CN110333194A
CN110333194A CN201910489142.1A CN201910489142A CN110333194A CN 110333194 A CN110333194 A CN 110333194A CN 201910489142 A CN201910489142 A CN 201910489142A CN 110333194 A CN110333194 A CN 110333194A
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tcnq
tetracyanoquinodimethane
quantitative analysis
concentration
carbon nano
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余皓
明静妍
曹永海
彭峰
王红娟
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South China University of Technology SCUT
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Abstract

The invention discloses a kind of methods of quantitative analysis carbon nano electronic transfer ability, comprising steps of (1) is in electrochemistry three-electrode system, fixed potential electrolysis certain time, preparation 7,7,8,8- tetracyanoquinodimethane (TCNQ) difference anion product pure material, the reference substance of configuration concentration gradient measures its ultraviolet-visible spectrum light absorption value, obtains the standard quantitative curve of different anion product light absorption values and concentration；(2) TCNQ is reacted into certain time in the acetonitrile of certain temperature with carbon nanotube, obtains TCNQ anion product, measure the ultraviolet-visible spectrum absorbance of supernatant；(3) concentration for reacting the TCNQ anion product generated is calculated with standard quantitative curve from absorbance, then the electron transfer number of carbon nanotube is obtained by calculation.The principle of the invention is simple, and universality is strong, is combined using spectrum analysis with electrochemistry preparation, can carry out quantization signifying to the electron transfer capacity of different carbon nanotubes.

Description

A kind of method of quantitative analysis carbon nano electronic transfer ability
Technical field
The invention belongs to carbon nanotube analysis technical fields more particularly to a kind of quantitative analysis carbon nano electronic to shift energy The method of power.
Technical background
Carbon nanotube has superior mechanics, electricity, optics and chemical property, obtains it in catalysis and electrochemical field Extensive concern and application.According to reported document, in liquid-phase catalytic oxidation, the surface electronic delocalization of carbon material Characteristic (i.e. electrodes transfer behaviour) plays a significant role its catalytic performance.It shows, is mixed by carbon material surface in the prior art Miscellaneous modification, introduce the means such as defect can effective its surface electronic characteristic of modulation, and then modulation its catalytic performance, and use UPS table Sign means are associated with carbon material surface characteristic electron and catalytic performance, can obtain better result, but can not still obtain more straight The data and method seen and can quantified.
Quantitative will be associated with qualitative electron transfer number with catalytic performance, which can probe into carbon-based catalysis material, is being catalyzed Important function played in system.At present still without related easy technique can the person of directing study realize this target, therefore, by carbon Material surface electrodes transfer behaviour carry out it is quantitative with it is qualitative be Recent study hot and difficult issue.It can be ground using spectral technique Study carefully the electron interaction between probe molecule and nitrating carbon nanomaterial, further analysis can be to carbon material surface electronics transfer Performance it is qualitative.Use the electricity such as tetracyanoethylene (TCNE), tetracyanoquinodimethane (TCNQ) and tetrathiafulvalene (TTF) Sub- probe and material surface interactions, then characterized with UV-Vis, it can be found that there are bright between nitrogen doped carbon nanotube and TCNQ Aobvious electrodes transfer behaviour, and the power of its interaction is influenced by the synthesis ratio of pyridine nitrogen and graphite nitrogen.According to nitrating Carbon nanotube and the feature absorbance of TCNQ electron transfer reaction liquid can define electron transfer interaction intensity.
In addition to carbon material, for utilizing electron acceptor tetracyanoethylene in the electrodes transfer behaviour research of metal material (TCNE) electrodes transfer behaviour of the different molybdenum oxide surface of reducing degree is studied, utilizes the absorption spectrum table of ionization TCNE Levy the electron transfer capacity of catalyst, the results showed that the electronics that the molybdenum oxide restored at 390 DEG C can provide is most.By partial reduction Molybdenum oxide as carrier loaded Au, it is found that the electronics on the surface Au catalyst Au of the molybdenum oxide load of 390 DEG C of reduction is more than needed most It is more, it is minimum in conjunction with energy position, and infrared spectroscopy red shift is most obvious.Electron acceptor TCNE and electricity are probed into using Raman Characterization Electron interaction between sub- donor TTF and boron-doping and nitrogen-doped graphene, it can be found that TCNE and TTF and boron-doping, nitrating When graphene interacts, the variation of the peak D of the two Raman spectrum and the frequency displacement direction at the peak 2G and half-peak breadth is all different, this It is caused by the difference of electronic structure characteristic due to caused by boron, N doping.
Above-mentioned all results of study show that electron probe molecule can be used as a kind of strong research means exploration carrier The characteristic of electronics transfer, but the work reported at present is only limitted to qualitative analysis to the research of electrodes transfer behaviour.Meanwhile passing through spy Needle molecule combination infrared spectroscopy with Raman spectra qualitative compared with electron transfer capacity height, have biggish uncertainty, Exact directive function cannot be played to liquid phase from now on, gas phase even electrocatalytic reaction.Therefore developing a kind of can accurately determine The method of amount analysis of catalyst surface electronic transfer ability is of great significance.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of method of quantitative analysis carbon nano electronic transfer ability. The present invention can be realized and accurately analyze different carbon nano electronic transfer performances, and the analysis method principle is simple, passes through experiment Room common instrument can meet, and have universality.
The purpose of the present invention is achieved through the following technical solutions.
A kind of method of quantitative analysis carbon nano electronic transfer ability, comprising the following steps:
(1) it is platinized platinum in working electrode, is carbon-point to electrode, reference electrode is silver/silver ion electrode three-electrode system In, potential electrolysis certain time, system are persistently fixed to certain density 7,7,8,8- tetracyanoquinodimethane acetonitrile solutions The acetonitrile solution of standby 7,7,8,8- tetracyanoquinodimethane difference anion product pure materials, the standard of configuration concentration gradient Object acetonitrile solution measures the ultraviolet-visible spectrum of 7,7,8,8- tetracyanoquinodimethane difference anion product pure materials Light absorption value obtains the standard quantitative curve of different anion product light absorption values and concentration；
(2) 7,7,8,8- tetracyanoquinodimethane (TCNQ) is reacted in the acetonitrile of certain temperature with carbon nanotube Certain time obtains 7,7,8,8- tetracyanoquinodimethane (TCNQ) anion products and measures its ultraviolet-visible spectrum Absorbance；
(3) from the ultraviolet-visible spectrum absorbance of step (2) from step (1) different anion product light absorption values with it is dense 7,7,8,8- tetracyanoquinodimethane (TCNQ) anion product that reaction generates is calculated in the standard quantitative curve of degree Concentration, then the electron transfer number of carbon nanotube is obtained by calculation.
Preferably, it is -0.3V vs Ag/Ag that current potential is fixed described in step (1)+Or -0.8V vs Ag/Ag+。
Preferably, TCNQ concentration needed for preparation described in step (1) is 0.1~1mmol/L, and the reaction time is 3~4h.
Preferably, the different anion product pure materials that generation is prepared described in step (1) are monovalent radical anion TCNQ.-, dianions oxidized derivatives DCTC-。
Preferably, configuration concentration gradient described in step (1) is 10-6~5 × 10-5mol/L。
Preferably, TCNQ reaction density described in step (2) is 1.56~6.24g/L, and carbon nanotube reaction density is 1.5 ~6.0g/L.
Preferably, carbon nanotube described in step (2) is carbon fluoride nano-tube or common carbon nanotube.
Preferably, certain temperature described in step (2) is 30~80 DEG C.
Preferably, the reaction time described in step (2) is 10~120min.
Preferably, the calculation method of electron transfer number described in step (3) is solution TCNQ after reaction.-Concentration adds twice DCTC-The sum of concentration is divided by the quality of addition carbon nanotube multiplied by Avogadro sieve constant (6.02 × 1023)。
Compared with the prior art, the invention has the following advantages:
1, the present invention prepares important and stable anion product using electrochemical method, obtains standard quantitative curve, ties Ultraviolet-visible spectrum is closed to different carbon nano electronic transfer performance qualitative analyses, finally obtains the accurate electronics of carbon nanotube Shift number.The principle of the invention is easily understood, and laboratory common instrument can be operated, and the electronics transfer of different carbon nanotubes can be obtained Number, it is strong for the universality of variety classes carbon nanotube, it is a kind of analysis method of the carbon nanotube of great popularization.
Detailed description of the invention
Fig. 1 is TCNQ.-The UV-visible spectrum of pure material.
Fig. 2 is DCTC-The UV-visible spectrum of pure material.
Fig. 3 is TCNQ.-The ultraviolet-visible spectrum light absorption value of pure material and the standard quantitative curve of concentration.
Fig. 4 is DCTC-The ultraviolet-visible spectrum light absorption value of pure material and the standard quantitative curve of concentration.
Specific embodiment
Specific implementation of the invention is further described below in conjunction with drawings and examples, but the present invention is not limited to Following embodiment.
Fluorine-containing carbon nanotube is labeled as FCNT, and after 600~1300 DEG C of argon annealeds handle 2h, F content can largely subtract It is few, it is left essentially C element, is respectively labeled as FCNT-600, FCNT-800, FCNT-900, FCNT-1100, FCNT-1300.
Common carbon nanotube is labeled as CNT, disperses in dehydrated alcohol with the six hydration cobalt acetates of 0wt%~12.5wt% Uniformly, naturally volatilize after in Muffle furnace 250 DEG C of calcining 30min, 2h is heated to reflux in concentrated nitric acid later, then in 800 DEG C of argons 2h is made annealing treatment in gas, obtains different degree of imperfection materials, is labeled as CNT-H-800, CNT-2Co-H-800, CNT-6Co-H- 800、CNT-12.5Co-H-800。
Embodiment 1
(1) in electrochemistry three-electrode system, working electrode is platinized platinum, to electrode be carbon-point, reference electrode be silver/silver from Sub-electrode persistently fixes current potential -0.3V vs Ag/Ag to 0.1mmol/L TCNQ acetonitrile solution+It is electrolysed 3h, is prepared 0.1mmol/L TCNQ.-The acetonitrile solution of pure material, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、5×10- 5The reference substance acetonitrile solution of mol/L, fixed current potential -0.8V vs Ag/Ag+It is electrolysed 3h, 0.1mmol/L DCTC is prepared-It is pure The acetonitrile solution of substance, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、3×10-5The reference substance acetonitrile of mol/L Solution measures its ultraviolet-visible spectrum light absorption value, as shown in Figure 1 and Figure 2, obtains different anion product light absorption values and concentration Standard quantitative curve, as shown in Figure 3, Figure 4.
Embodiment 2-6
(1) in electrochemistry three-electrode system, working electrode is platinized platinum, to electrode be carbon-point, reference electrode be silver/silver from Sub-electrode persistently fixes current potential -0.3V vs Ag/Ag to 1mmol/L TCNQ acetonitrile solution+It is electrolysed 4h, 1mmol/ is prepared L TCNQ.-The acetonitrile solution of pure material, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、5×10-5The mark of mol/L Quasi- object acetonitrile solution, fixed current potential -0.8V vs Ag/Ag+It is electrolysed 4h, 1mmol/L DCTC is prepared-The acetonitrile of pure material is molten Liquid, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、3×10-5The reference substance acetonitrile solution of mol/L measures its purple Outside-visible spectrum light absorption value obtains the standard quantitative curve of different anion product light absorption values and concentration.
(2) by 1.56g/L 7,7,8,8- tetracyanoquinodimethane (TCNQ) and 1.5g/L FCNT-800 at 80 DEG C 10,20,60,90,120min are reacted in acetonitrile, obtain 7,7,8,8- tetracyanoquinodimethane (TCNQ) anion products, The ultraviolet-visible spectrum absorbance of supernatant is measured, as shown in table 1.
The absorbance of differential responses time in 1 embodiment 2-6 of table
(3) 7,7,8,8- for reacting and generating is calculated with the standard quantitative curve of step (1) from the absorbance of step (2) The concentration of tetracyanoquinodimethane (TCNQ) anion product, then the electron transfer number of carbon nanotube is obtained by calculation.
The transfer electron number of differential responses time in 2 embodiment 2-6 of table
1.56g/L TCNQ and 1.5g/L FCNT-800 can be obtained in the differential responses time by table 2, the electronics of carbon nanotube turns It is different to move number.At a certain temperature, in per unit volume acetonitrile, the electron number of per unit mass carbon nanotube transfer is with the time Increase and increases.
Embodiment 7-11
(1) in electrochemistry three-electrode system, working electrode is platinized platinum, to electrode be carbon-point, reference electrode be silver/silver from Sub-electrode persistently fixes current potential -0.3V vs Ag/Ag to 1mmol/L TCNQ acetonitrile solution+It is electrolysed 4h, 1mmol/ is prepared L TCNQ.-The acetonitrile solution of pure material, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、5×10-5The mark of mol/L Quasi- object acetonitrile solution, fixed current potential -0.8V vs Ag/Ag+It is electrolysed 4h, 1mmol/L DCTC is prepared-The acetonitrile of pure material is molten Liquid, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、3×10-5The reference substance acetonitrile solution of mol/L measures its purple Outside-visible spectrum light absorption value obtains the standard quantitative curve of different anion product light absorption values and concentration.
(2) by 6.24g/L 7,7,8,8- tetracyanoquinodimethane (TCNQ) and 1.5g/L FCNT-800 at 80 DEG C 10,20,60,90,120min are reacted in acetonitrile, obtain 7,7,8,8- tetracyanoquinodimethane (TCNQ) anion products, The ultraviolet-visible spectrum absorbance of supernatant is measured, as shown in table 3.
The absorbance of differential responses time in 3 embodiment 7-11 of table
(3) 7,7,8,8- for reacting and generating is calculated with the standard quantitative curve of step (1) from the absorbance of step (2) The concentration of tetracyanoquinodimethane (TCNQ) anion product, then the electron transfer number of carbon nanotube is obtained by calculation.
The transfer electron number of differential responses time in 4 embodiment 7-11 of table
6.24g/L TCNQ and 1.5g/L FCNT-800 can be obtained in the differential responses time by table 4, the electronics of carbon nanotube turns It is different to move number.At a certain temperature, in per unit volume acetonitrile, the electron number of per unit mass carbon nanotube transfer is with the time Increase and increases.
Embodiment 12-15
(1) in electrochemistry three-electrode system, working electrode is platinized platinum, to electrode be carbon-point, reference electrode be silver/silver from Sub-electrode persistently fixes current potential -0.3V vs Ag/Ag to 1mmol/L TCNQ acetonitrile solution+It is electrolysed 4h, 1mmol/ is prepared L TCNQ.-The acetonitrile solution of pure material, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、5×10-5The mark of mol/L Quasi- object acetonitrile solution, fixed current potential -0.8V vs Ag/Ag+It is electrolysed 4h, 1mmol/L DCTC is prepared-The acetonitrile of pure material is molten Liquid, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、3×10-5The reference substance acetonitrile solution of mol/L measures its purple Outside-visible spectrum light absorption value obtains the standard quantitative curve of different anion product light absorption values and concentration.
(2) by 1.56g/L 7,7,8,8- tetracyanoquinodimethane (TCNQ) and 1.5,3,4.5,6g/LFCNT-800 10,20,60,90,120min are reacted in 80 DEG C of acetonitriles, obtain 7,7,8,8- tetracyanoquinodimethane (TCNQ) anions Product measures the ultraviolet-visible spectrum absorbance of supernatant, as shown in table 5.
The absorbance of differential responses object concentration in 5 embodiment 12-15 of table
(3) 7,7,8,8- for reacting and generating is calculated with the standard quantitative curve of step (1) from the absorbance of step (2) The concentration of tetracyanoquinodimethane (TCNQ) anion product, then the electron transfer number of carbon nanotube is obtained by calculation.
The transfer electron number of differential responses object concentration in 6 embodiment 12-15 of table
1.56g/L 7,7,8,8- tetracyanoquinodimethane (TCNQ) and 1.5,3,4.5,6g/ can be obtained by table 6 LFCNT-800 carbon nanotube electron transfer number it is different.At a certain temperature, in per unit volume acetonitrile, per unit matter The electron number of amount carbon nanotube transfer increases as reactant concentration increases.
Embodiment 16-20
(1) in electrochemistry three-electrode system, working electrode is platinized platinum, to electrode be carbon-point, reference electrode be silver/silver from Sub-electrode persistently fixes current potential -0.3V vs Ag/Ag to 1mmol/L TCNQ acetonitrile solution+It is electrolysed 4h, 1mmol/ is prepared L TCNQ.-The acetonitrile solution of pure material, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、5×10-5The mark of mol/L Quasi- object acetonitrile solution, fixed current potential -0.8V vs Ag/Ag+It is electrolysed 4h, 1mmol/L DCTC is prepared-The acetonitrile of pure material is molten Liquid, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、3×10-5The reference substance acetonitrile solution of mol/L measures its purple Outside-visible spectrum light absorption value obtains the standard quantitative curve of different anion product light absorption values and concentration.
(2) by 1.56g/L 7,7,8,8- tetracyanoquinodimethane (TCNQ) and 1.5g/L FCNT-600, FCNT- 800, FCNT-900, FCNT-1100, FCNT-1300 react 20min in 80 DEG C of acetonitriles, obtain 7,7,8,8- four cyanos to benzene Quinone bismethane (TCNQ) anion product, measures the ultraviolet-visible spectrum absorbance of supernatant, as shown in table 7.
The absorbance of FCNT different annealing temperature in 7 embodiment 16-20 of table
(3) 7,7,8,8- for reacting and generating is calculated with the standard quantitative curve of step (1) from the absorbance of step (2) The concentration of tetracyanoquinodimethane (TCNQ) anion product, then the electron transfer number of carbon nanotube is obtained by calculation.
The transfer electron number of FCNT different annealing temperature in 8 embodiment 16-20 of table
Different annealing temperature can be obtained treated fluorine-containing carbon pipe by table 8, surface functional group content is different, and degree of imperfection is not yet Together, so that the electronics transfer property shown is also different.Under certain temperature and reaction time, in per unit volume acetonitrile, often The electron number of unit mass FCNT-900 transfer is most, and FCNT-600 is because containing having electrophilic F element on a small quantity, transfer is electric Sub- property shows as electrophilic.
Embodiment 21-24
(1) in electrochemistry three-electrode system, working electrode is platinized platinum, to electrode be carbon-point, reference electrode be silver/silver from Sub-electrode persistently fixes current potential -0.3V vs Ag/Ag to 1mmol/L TCNQ acetonitrile solution+It is electrolysed 4h, 1mmol/ is prepared L TCNQ.-The acetonitrile solution of pure material, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、5×10-5The mark of mol/L Quasi- object acetonitrile solution, fixed current potential -0.8V vs Ag/Ag+It is electrolysed 4h, 1mmol/L DCTC is prepared-The acetonitrile of pure material is molten Liquid, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、3×10-5The reference substance acetonitrile solution of mol/L measures its purple Outside-visible spectrum light absorption value obtains the standard quantitative curve of different anion product light absorption values and concentration.
(2) by 1.56g/L 7,7,8,8- tetracyanoquinodimethane (TCNQ) and 1.5g/L CNT-H-800, CNT- 2Co-H-800,CNT-6Co-H-800,CNT-12.5Co-H-800.20min is reacted in 80 DEG C of acetonitriles, obtains 7,7,8,8- tetra- Cyano 1,4-benzoquinone bismethane (TCNQ) anion product, measures the ultraviolet-visible spectrum absorbance of supernatant, as shown in table 9.
The absorbance of difference CNT material in 9 embodiment 21-24 of table
(3) 7,7,8,8- for reacting and generating is calculated with the standard quantitative curve of step (1) from the absorbance of step (2) The concentration of tetracyanoquinodimethane (TCNQ) anion product, then the electron transfer number of carbon nanotube is obtained by calculation.
The transfer electron number of difference CNT material in 10 embodiment 21-24 of table
Different cobalt contents can be obtained treated carbon nanotube by table 10, degree of imperfection is different, so that the electronics shown turns It is also different to move property.Under certain temperature and reaction time, in per unit volume acetonitrile, what per unit mass carbon nanotube was added Cobalt content is higher, and degree of imperfection is higher, then the electron number shifted is most.
Embodiment 25-28
(1) in electrochemistry three-electrode system, working electrode is platinized platinum, to electrode be carbon-point, reference electrode be silver/silver from Sub-electrode persistently fixes current potential -0.3V vs Ag/Ag to 1mmol/L TCNQ acetonitrile solution+It is electrolysed 4h, 1mmol/ is prepared L TCNQ.-The acetonitrile solution of pure material, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、5×10-5The mark of mol/L Quasi- object acetonitrile solution, fixed current potential -0.8V vs Ag/Ag+It is electrolysed 4h, 1mmol/L DCTC is prepared-The acetonitrile of pure material is molten Liquid, configuration concentration gradient are 10-6、5×10-6、10-5、2×10-5、3×10-5The reference substance acetonitrile solution of mol/L measures its purple Outside-visible spectrum light absorption value obtains the standard quantitative curve of different anion product light absorption values and concentration.
(2) by 1.56g/L 7,7,8,8- tetracyanoquinodimethane (TCNQ) and 1.5g/L FCNT-800 30, 40,20min is reacted in 60,80 DEG C of acetonitriles, obtains 7,7,8,8- tetracyanoquinodimethane (TCNQ) anion products, measured The ultraviolet-visible spectrum absorbance of supernatant, as shown in table 11.
The absorbance of differential responses temperature in 11 embodiment 25-28 of table
(3) 7,7,8,8- for reacting and generating is calculated with the standard quantitative curve of step (1) from the absorbance of step (2) The concentration of tetracyanoquinodimethane (TCNQ) anion product, then the electron transfer number of carbon nanotube is obtained by calculation.
The transfer electron number of differential responses temperature in 12 embodiment 25-28 of table
1.56g/L TCNQ can be obtained from 1.5g/L FCNT-800 in different anti-temperature by table 12, the electronics of carbon nanotube turns It is different to move number.In certain time, in per unit volume acetonitrile, the electron number of per unit mass carbon nanotube transfer is with reaction Temperature increases and increases.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (10)

1. a kind of method of quantitative analysis carbon nano electronic transfer ability, which comprises the following steps:
(1) working electrode be platinized platinum, to electrode be carbon-point, reference electrode be silver/silver ion electrode three-electrode system in, it is right Certain density 7,7,8,8- tetracyanoquinodimethane acetonitrile solutions persistently fix potential electrolysis certain time, prepare 7,7, The acetonitrile solution of 8,8- tetracyanoquinodimethane difference anion product pure materials, the reference substance acetonitrile of configuration concentration gradient Solution measures the ultraviolet-visible spectrum light absorption value of 7,7,8,8- tetracyanoquinodimethane difference anion product pure materials, Obtain the standard quantitative curve of different anion product light absorption values and concentration；
(2) 7,7,8,8- tetracyanoquinodimethanes are reacted into certain time in the acetonitrile of certain temperature with carbon nanotube, It obtains 7,7,8,8- tetracyanoquinodimethane anion product and measures its ultraviolet-visible spectrum absorbance；
(3) from the ultraviolet-visible spectrum absorbance of step (2) anion product light absorption value different from step (1) and concentration The concentration for 7,7,8, the 8- tetracyanoquinodimethane anion products that reaction generates is calculated in standard quantitative curve, then leads to Cross the electron transfer number that carbon nanotube is calculated in formula.
2. a kind of method of quantitative analysis carbon nano electronic transfer ability according to claim 1, which is characterized in that step Suddenly it is -0.3V vs Ag/Ag that current potential is fixed described in (1)+Or -0.8V vs Ag/Ag+。
3. a kind of method of quantitative analysis carbon nano electronic transfer ability according to claim 1, which is characterized in that step Suddenly described in (1) preparation needed for 7,7,8,8- tetracyanoquinodimethane concentration be 0.1~1mmol/L, the reaction time be 3~ 4h。
4. a kind of method of quantitative analysis carbon nano electronic transfer ability according to claim 1, which is characterized in that step Suddenly the 7,7,8,8- tetracyanoquinodimethane difference anion product pure material that generation is prepared described in (1) is that monovalence is free Base anion TCNQ.-, dianions oxidized derivatives DCTC-。
5. a kind of method of quantitative analysis carbon nano electronic transfer ability according to claim 1, which is characterized in that step Suddenly configuration concentration gradient described in (1) is 10-6~5 × 10-5mol/L。
6. a kind of method of quantitative analysis carbon nano electronic transfer ability according to claim 1, which is characterized in that step Suddenly 7,7,8,8- tetracyanoquinodimethane reaction densities described in (2) are 1.56~6.24g/L, carbon nanotube reaction density For 1.5~6.0g/L.
7. a kind of method of quantitative analysis carbon nano electronic transfer ability according to claim 1, which is characterized in that step Suddenly carbon nanotube described in (2) is carbon fluoride nano-tube or common carbon nanotube.
8. a kind of method of quantitative analysis carbon nano electronic transfer ability according to claim 1, which is characterized in that step Suddenly certain temperature described in (2) is 30~80 DEG C.
9. a kind of method of quantitative analysis carbon nano electronic transfer ability according to claim 1, which is characterized in that step Suddenly the reaction time described in (2) is 10~120min.
10. a kind of method of quantitative analysis carbon nano electronic transfer ability according to claim 1, which is characterized in that The calculation method of electron transfer number described in step (3) is solution TCNQ after reaction.-Concentration adds twice of DCTC-The sum of concentration Divided by the quality of addition carbon nanotube multiplied by Avogadro sieve constant.
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CN1448396A (en) * 2003-04-25 2003-10-15 中国科学院上海光学精密机械研究所 Copper-tetracyano-p-benzoquinone dimethane ester derivative and synthesis method thereof
CN1460680A (en) * 2003-06-13 2003-12-10 中国科学院上海光学精密机械研究所 Synthesis method of metal-tetracyano-p-benzoquinone dimethane ester derivatives

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CN1460680A (en) * 2003-06-13 2003-12-10 中国科学院上海光学精密机械研究所 Synthesis method of metal-tetracyano-p-benzoquinone dimethane ester derivatives

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