CN108928809A - The fluorine carbon ratio of carbon fluoride nano-tube regulates and controls method - Google Patents
The fluorine carbon ratio of carbon fluoride nano-tube regulates and controls method Download PDFInfo
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- CN108928809A CN108928809A CN201710363771.0A CN201710363771A CN108928809A CN 108928809 A CN108928809 A CN 108928809A CN 201710363771 A CN201710363771 A CN 201710363771A CN 108928809 A CN108928809 A CN 108928809A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
- C01P2004/133—Multiwall nanotubes
Abstract
The present invention discloses the fluorine carbon ratio regulation method of carbon fluoride nano-tube, carbon fluoride nano-tube and polar solvent are heated up after mixing and reacted, fluorine element in carbon nanotube is replaced with polar solvent, so that fluorine atom is detached from from carbon pipe, or active force between reduction carbon fluorine, reach fluorine effect.The present invention can control the defluorinate amount of carbon pipe, to control the fluorine carbon ratio of carbon fluoride nano-tube by selecting different polar solvent, hydrothermal temperature and hydro-thermal time very well, it is easy to operate, degree of controllability is high, can be reduced carbon pipe structure compared to the high temperature anneal and destroys, keeps carbon pipe excellent properties itself.
Description
Technical field
The present invention relates to a kind of preparation methods of the carbon fluoride nano-tube of controllable fluorine carbon ratio, are more particularly to pass through pole
Property solvent carries out fluorine to the fluorination multi-walled carbon nanotube of high fluorine amount to adjust fluorine carbon ratio.
Background technique
With the development of electronics technology, electronic product plays an important role in human lives, and battery performance
Quality directly affects the usage experience of people, therefore develops stabilization, safety, intelligence and sustainable battery and seem and especially close
Key.In all energy storage materials, fluorocarbons gets more and more people's extensive concerning as battery material specific energy with higher.Fluorine
Carbon nano tube, which compares the fluorographite studied in the past, has higher discharge voltage and high rate performance, and development prospect is wide.But
The fluorine carbon ratio of gaseous fluoridizing method fluorination multi-walled carbon nanotube obtained is not easy to control, can not achieve the accuracy controlling of fluorine carbon ratio, because
This needs to prepare the fluorination multi-walled carbon nanotube of different fluorine carbon ratios by subsequent solution processing, regulates and controls battery performance.
Carbon nano tube structure stablize, high mechanical strength, large specific surface area, good conductivity, have excellent mechanics, optics,
Electricity and chemical property are constantly mined discovery using potentiality.By the way that multi-walled carbon nanotube is fluorinated and can greatly be changed
It is apt to its performance, there is important application on electrode material.Become using thus battery material is prepared using carbon fluoride nano-tube material
Also there is the authorization of similar patent or openly in the research emphasis of people.State Intellectual Property Office of the People's Republic of China's grant number
It is disclosed for patents of invention such as CN2010101023873A, CN102730664A, CN103700858A standby using fluorocarbons control
The technology of electrode material.The above patent of invention discloses only the preparation method of fluorocarbons pipe, using gaseous fluoridizing method how
The outer surface of carbon pipe connects fluorine atom.For being fluorinated multi-walled carbon nanotube, fluorine gas reactivity is very strong, by opening the π on carbon pipe
Key forms C-F key in conjunction with carbon atom.Tradition goes fluorine technique using high annealing, and fluorine atom is broken at high temperature with volatile matter
Form diffusion, the tubular structure of carbon pipe may be destroyed while reducing fluorine carbon ratio.
Summary of the invention
The present invention is not easy the shortcomings that accurately controlling fluorine carbon ratio for carbon fluoride nano-tube technique, provides a kind of polar solvent
The preparation method of the carbon fluoride nano-tube of post-processing regulation fluorine carbon ratio, and with polar solvent at low temperature to fluorination multi-wall carbon nano-tube
Pipe carries out fluorine carbon ratio regulation, and carbon pipe structure can be made by smaller destruction, maintain higher electronic conductivity, and then change C-F
Covalent bond and ionic bond ratio can regulate and control its structure and electrology characteristic in a wide range.Therefore, in fluorination (multi wall) carbon
It on the basis of the existing advantage of nano-tube material, is post-processed with polar solvent, the mesh for effectively controlling its fluorine carbon ratio can be reached
, important experiment and theories integration are provided to study the chemical property rule of multi-wall carbon tube of different fluorine carbon ratios.
Technical purpose of the invention is achieved by following technical proposals：
The fluorine carbon ratio of carbon fluoride nano-tube regulates and controls method, and carbon fluoride nano-tube and polar solvent are uniformly mixed and are placed on water
It is sealed in hot kettle, 120~180 DEG C and insulation reaction is warming up in air atmosphere.
In the above-mentioned technical solutions, carbon fluoride nano-tube hydro-thermal finished, which pours into sand core funnel, to be filtered, and deionization is used
Water repeatedly washs, and until cleaning up, filter membrane is then transferred to culture dish, is placed in a vacuum drying oven, under the conditions of 60 DEG C
Drying is for 24 hours.
In the above-mentioned technical solutions, by carbon fluoride nano-tube and polar solvent 1~3h of ultrasound, to be uniformly mixed, from room temperature
20-25 degrees Celsius with 1-5 degrees Celsius per minute of speed be warming up to 120~180 DEG C and keep the temperature 18~for 24 hours, preferably 140-
160 degrees Celsius insulation reaction 20-24 hours.
In the above-mentioned technical solutions, carbon fluoride nano-tube is fluorination multi-walled carbon nanotube, mole of fluorine element and carbon
Than being 1：1.
In the above-mentioned technical solutions, polar solvent is isopropanol, tetrahydrofuran, ethylene glycol or propylene glycol.
In the above-mentioned technical solutions, the ratio of the parts by volume (ml) of the mass parts (mg) and polar solvent of carbon fluoride nano-tube
It is 1：(1-1.5), preferably 1：(1-1.2), such as carbon fluoride nano-tube dosage are 60~120mg, polar solvent volume (mL)
It is the 100%~150% of fluorination multi-walled carbon nanotube quality.
In technical solution of the present invention, hydrothermal system is formed by carbon fluoride nano-tube and polar solvent, in hydrothermal solution system
In, the Bronsted acid (H of polar solvent+) fluorine atom on carbon pipe is acted on, or the fluorine atom on carbon pipe is replaced, fluorine
Atom is detached from from carbon pipe, or (such as carbon fluorine covalent bond is changed into half ion to the active force between reduction fluorine atom and carbon atom
Key or ionic bond), reach the technical effect of fluorine.Simultaneously by selecting different polar solvent, hydrothermal temperature and water
The usage ratio of thermal response time and carbon nanotube and polar solvent can control the defluorinate amount of carbon pipe, to control very well
The fluorine carbon ratio of carbon fluoride nano-tube.Selecting fluorination multi-walled carbon nanotube in embodiment is raw material, and fluorine carbon ratio example is 1, is being carried out
After the hydrothermal experiment of different technology conditions, fluorine carbon ratio example is changed and (is tested using EDS) in product；It is microcosmic next from product
It sees, carbon nanotube pattern is not significantly affected, from the point of view of product appearance observation, fluorination multi-walled carbon nanotube entirety burnt hair hair
White, after reducing fluorine element content using technical solution of the present invention, carbon pipe apparently gradually becomes black.
Compared with prior art, the present invention provides a kind of polar solvents to be aided with low-temperature heat regulation carbon nanotube fluorine carbon ratio
Preparation method, easy to operate, degree of controllability is high, can be reduced carbon pipe structure compared to the high temperature anneal and destroys, keeps carbon pipe itself
Excellent properties, the carbon pipe of the different fluorine carbon ratios of technical solution preparation can be used for regulating and controlling battery performance according to the present invention, to research fluorine
Carbon ratio influences meaningful (i.e. fluorine carbon ratio regulation method the answering in regulation battery performance of carbon fluoride nano-tube to battery performance
With, i.e., it will be without the carbon fluoride nano-tube of fluorine carbon ratio as electrode material, assembled battery, based on not having to, fluorine carbon ratio realization is cell performance
The regulation of energy).
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture for the fluorination multi-walled carbon nanotube that the embodiment of the present invention uses.
Fig. 2 is the XPS spectrum figure for the fluorination multi-walled carbon nanotube that the embodiment of the present invention uses.
Fig. 3 is the stereoscan photograph that the multi-wall carbon tube after fluorine is removed using technical solution of the present invention.
Fig. 4 is that the EDS of the multi-wall carbon tube after fluorine is gone to test spectrogram using technical solution of the present invention.
Specific embodiment
6 embodiments of the invention are given below, are that rather than model of the invention is limited to further explanation of the invention
It encloses.The use of fluorination multi-walled carbon nanotube is in embodiment that raw material carries out the adjustment of fluorine carbon ratio example, is fluorinated multi-walled carbon nanotube (fluorine carbon
Than for preparation method 1)：Multi-walled carbon nanotube is put in monel metal reaction kettle, fluorine gas percentage by volume 20% is passed through
F2/N2Mixed gas reacts 8h at 400 DEG C, carries out depth fluorination, detects through EDS, obtains the fluorination multi wall carbon that fluorine carbon ratio is 1
Nanotube.
Embodiment 1
60g is fluorinated multi-walled carbon nanotube and 80mL isopropanol uniformly mixes, then dispersion liquid is transferred to water by ultrasonic 1h
In hot kettle, it is warming up to 130 DEG C in Muffle furnace and keeps the temperature for 24 hours；The fluorination multi-walled carbon nanotube that hydro-thermal finishes is poured into sand core leakage
It is filtered in bucket, is repeatedly washed with deionized water, until cleaning up, filter membrane is then transferred to culture dish, it is dry to be placed on vacuum
In dry case, dried for 24 hours under the conditions of 60 DEG C.The fluorine carbon ratio for measuring fluorination multi-walled carbon nanotube is 0.65.
Embodiment 2
80g is fluorinated multi-walled carbon nanotube and 80mL tetrahydrofuran uniformly mixes, then dispersion liquid is transferred to by ultrasonic 2h
In water heating kettle, it is warming up to 150 DEG C in Muffle furnace and keeps the temperature for 24 hours；The fluorination multi-walled carbon nanotube that hydro-thermal finishes is poured into sand core
It is filtered in funnel, is repeatedly washed with deionized water, until cleaning up, filter membrane is then transferred to culture dish, is placed on vacuum
In drying box, dried for 24 hours under the conditions of 60 DEG C.The fluorine carbon ratio for measuring fluorination multi-walled carbon nanotube is 0.59.
Embodiment 3
80g is fluorinated multi-walled carbon nanotube and 80mL ethylene glycol uniformly mixes, then dispersion liquid is transferred to water by ultrasonic 2h
In hot kettle, it is warming up to 150 DEG C in Muffle furnace and keeps the temperature for 24 hours；The fluorination multi-walled carbon nanotube that hydro-thermal finishes is poured into sand core leakage
It is filtered in bucket, is repeatedly washed with deionized water, until cleaning up, filter membrane is then transferred to culture dish, it is dry to be placed on vacuum
In dry case, dried for 24 hours under the conditions of 60 DEG C.The fluorine carbon ratio for measuring fluorination multi-walled carbon nanotube is 0.76.
Embodiment 4
80g is fluorinated multi-walled carbon nanotube and 80mL propylene glycol uniformly mixes, then dispersion liquid is transferred to water by ultrasonic 2h
In hot kettle, it is warming up to 150 DEG C in Muffle furnace and keeps the temperature for 24 hours；The fluorination multi-walled carbon nanotube that hydro-thermal finishes is poured into sand core leakage
It is filtered in bucket, is repeatedly washed with deionized water, until cleaning up, filter membrane is then transferred to culture dish, it is dry to be placed on vacuum
In dry case, dried for 24 hours under the conditions of 60 DEG C.The fluorine carbon ratio for measuring fluorination multi-walled carbon nanotube is 0.56.
Embodiment 5
100g is fluorinated multi-walled carbon nanotube and 120mL isopropanol uniformly mixes, then dispersion liquid is transferred to by ultrasonic 3h
In water heating kettle, it is warming up to 180 DEG C in Muffle furnace and keeps the temperature for 24 hours；The fluorination multi-walled carbon nanotube that hydro-thermal finishes is poured into sand core
It is filtered in funnel, is repeatedly washed with deionized water, until cleaning up, filter membrane is then transferred to culture dish, is placed on vacuum
In drying box, dried for 24 hours under the conditions of 60 DEG C.The fluorine carbon ratio for measuring fluorination multi-walled carbon nanotube is 0.61.
Embodiment 6
100g is fluorinated multi-walled carbon nanotube and 120mL propylene glycol uniformly mixes, then dispersion liquid is transferred to by ultrasonic 3h
In water heating kettle, it is warming up to 180 DEG C in Muffle furnace and keeps the temperature for 24 hours；The fluorination multi-walled carbon nanotube that hydro-thermal finishes is poured into sand core
It is filtered in funnel, is repeatedly washed with deionized water, until cleaning up, filter membrane is then transferred to culture dish, is placed on vacuum
In drying box, dried for 24 hours under the conditions of 60 DEG C.The fluorine carbon ratio for measuring fluorination multi-walled carbon nanotube is 0.50.
The adjustment of technological parameter is carried out according to the content of present invention, it can be for fluorine element and carbon ratio in carbon nanotube
It is adjusted.Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (7)
1. the fluorine carbon ratio of carbon fluoride nano-tube regulates and controls method, which is characterized in that mix carbon fluoride nano-tube and polar solvent equal
Even be placed in water heating kettle seals, and 120~180 DEG C and insulation reaction are warming up in air atmosphere；By carbon fluoride nano-tube and
Polar solvent forms hydrothermal system, and in hydrothermal solution system, the Bronsted acid of polar solvent makees the fluorine atom on carbon pipe
With, or the fluorine atom on carbon pipe replaced, fluorine atom is detached from from carbon pipe, or between reduction fluorine atom and carbon atom
Active force reaches the technical effect of fluorine.
2. the fluorine carbon ratio of carbon fluoride nano-tube according to claim 1 regulates and controls method, which is characterized in that polar solvent is different
Propyl alcohol, tetrahydrofuran, ethylene glycol or propylene glycol.
3. the fluorine carbon ratio of carbon fluoride nano-tube according to claim 1 regulates and controls method, which is characterized in that carbon fluoride nano-tube
Mass parts (mg) and polar solvent parts by volume (ml) ratio be 1：(1-1.5), preferably 1：(1—1.2).
4. the fluorine carbon ratio of carbon fluoride nano-tube according to claim 1 regulates and controls method, which is characterized in that by fluorocarbons nanometer
Pipe and 1~3h of polar solvent ultrasound, to be uniformly mixed, from 20-25 degrees Celsius of room temperature with 1-5 degrees Celsius per minute of speed liter
Temperature to 120~180 DEG C and keep the temperature 18~for 24 hours, preferably 140-160 degrees Celsius insulation reaction 20-24 hours.
5. the fluorine carbon ratio of carbon fluoride nano-tube according to claim 1 regulates and controls method, which is characterized in that carbon fluoride nano-tube
For fluorination multi-walled carbon nanotube, the molar ratio of fluorine element and carbon is 1：1.
6. the fluorine carbon ratio of carbon fluoride nano-tube according to claim 1 regulates and controls method, which is characterized in that different by selecting
Polar solvent, hydrothermal temperature and the hydro-thermal reaction time and carbon nanotube and polar solvent usage ratio, control carbon
The defluorinate amount of pipe, to control the fluorine carbon ratio of carbon fluoride nano-tube.
7. the fluorine carbon ratio regulation method of the carbon fluoride nano-tube as described in one of claim 1-6 is in regulation battery performance
Using.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112038650A (en) * | 2020-07-28 | 2020-12-04 | 天津力神电池股份有限公司 | Flexible package lithium fluorocarbon primary battery |
| CN113233443A (en) * | 2021-04-22 | 2021-08-10 | 电子科技大学 | Preparation method of fluorinated spiral carbon nanotube and application of fluorinated spiral carbon nanotube in lithium primary battery |
| CN114583128A (en) * | 2022-03-07 | 2022-06-03 | 湘潭大学 | Controllable preparation method of surface high-conductivity carbon fluoride |
| CN114628631A (en) * | 2022-03-07 | 2022-06-14 | 湘潭大学 | Preparation method of high-capacity alkali metal-carbon fluoride secondary battery |
| CN115124029A (en) * | 2022-07-22 | 2022-09-30 | 电子科技大学 | Preparation method of precise carbon fluoride nanotube array and application of lithium primary battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112038650A (en) * | 2020-07-28 | 2020-12-04 | 天津力神电池股份有限公司 | Flexible package lithium fluorocarbon primary battery |
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| CN114628631B (en) * | 2022-03-07 | 2023-09-19 | 湘潭大学 | Preparation method of high-capacity alkali metal-carbon fluoride secondary battery |
| CN114583128B (en) * | 2022-03-07 | 2023-09-19 | 湘潭大学 | Controllable preparation method of surface highly conductive carbon fluoride |
| CN115124029A (en) * | 2022-07-22 | 2022-09-30 | 电子科技大学 | Preparation method of precise carbon fluoride nanotube array and application of lithium primary battery |
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Application publication date: 20181204 |