CN106252632A - A kind of carbon fiber and the preparation method of stibium oxide composite - Google Patents
A kind of carbon fiber and the preparation method of stibium oxide composite Download PDFInfo
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- CN106252632A CN106252632A CN201610828356.3A CN201610828356A CN106252632A CN 106252632 A CN106252632 A CN 106252632A CN 201610828356 A CN201610828356 A CN 201610828356A CN 106252632 A CN106252632 A CN 106252632A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
A kind of carbon fiber and the preparation method of stibium oxide composite, take analytically pure CTAB and be dissolved completely in analytically pure ethanol, add SbCl under stirring3Obtain uniform solution A；Take in carbon fiber addition solution A and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8～9；B solution is placed in temperature control baking oven and carries out solvent thermal reaction and obtain sample, samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and stibium oxide composite in oven for drying；The present invention uses solvent-thermal method to prepare sodium-ion battery anode material Cf‑Sb2O3, temperature is relatively low, simple to operate easy to control；The C prepared by the inventive methodf‑Sb2O3Composite chemical composition is homogeneous, and purity is higher, good crystallinity, and pattern is homogeneous, grown on carbon fibers stably the most square phase Sb2O3, this product has been effectively combined carbon fiber and stibium oxide advantage, has had higher specific capacity the most simultaneously, keep again preferable cycle characteristics.
Description
Technical field
The invention belongs to field of material preparation, be specifically related to a kind of carbon fiber and stibium oxide composite (Cf-Sb2O3)
Preparation method.
Background technology
As far back as the eighties in 20th century, lithium ion battery is just widely studied, along with lithium ion battery successful commercialization, sodium from
Sub-battery is the most studied.Sodium and lithium belong to same main group, have similar physicochemical property, battery charging and discharging principle basic
Cause.Compared with lithium ion battery, sodium-ion battery has the following characteristics that sodium aboundresources, accounts for crustal elements reserves
2.64%, and cheap, widely distributed.Sodium ion is utilized to realize the accumulator repeatedly charged, discharge, owing to sodium resource is stored up
Amount is abundant and easily realizes low-cost production, is considered as substituting the accumulator of future generation of lithium ion battery by part expert.
Sb2O3It is that one has the half of quantum size effect, small-size effect, skin effect and macro quanta tunnel effect
Conductor, the distinctive effect of these quasiconductors so that it is show many macroscopic views ins and outs not available for block materials.Sb2O3Receive
Rice semi-conducting material band gap is the least, and under relatively low electric field intensity, electronics just can reach saturation drift velocity, has excellent
Good photoelectric conversion characteristic, higher charge transfer speed, steady in a long-term, respond rapid, reproducible, cheap,
Theoretical specific capacity, up to 1103mAh/g, presents tempting application prospect in field of batteries.
Carbon fiber is the tencel material of a kind of phosphorus content high intensity more than 95%, high modulus fibre.It is by
The organic fibers such as flake graphite crystallite are piled up along fiber axial direction and are formed, the microlite obtained through carbonization and graphitization processing
Ink material.It not only has the intrinsic intrinsic property of material with carbon element, has both again the soft machinability of textile fabric, is that a new generation increases
Strong fiber.Carbon fiber has many premium properties, and the axial strength of carbon fiber and modulus are high, and density is low, higher than performance, without compacted
Becoming, superhigh temperature resistant under non-oxidizing atmosphere, fatigue durability is good, specific heat and electric conductivity between nonmetal and metal, thermal expansion system
Number is little and has anisotropy, good corrosion resistance, and X-ray transparent is good, and good electrical and thermal conductivity performance, electromagnetic wave shielding are good
Deng.
Some researchs show, by Sb2O3By compound being likely to be obtained of proper method, there is Sb with material with carbon element2O3And material with carbon element
The new material of advantage, has higher specific capacity the most simultaneously and keeps again preferable cycle characteristics.
Summary of the invention:
Technical process is simple, reaction time is short, materials chemistry forms homogeneous, pattern to it is an object of the invention to provide one
The preparation method of size uniform and the preferable carbon fiber of cyclical stability and stibium oxide composite.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
1) take the analytically pure CTAB of 0.15-0.2g to be dissolved completely in the analytically pure ethanol of 30-40ml, will in whipping process
The SbCl of 0.85-1.14g3Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2-3g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8～9；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 20 DEG C-100 DEG C, the time
For 2h-10h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and oxygen in oven for drying
Change antimony composite.
The present invention uses solvent-thermal method to prepare sodium-ion battery anode material Cf-Sb2O3, temperature is relatively low, simple to operate easily-controllable
System.The C prepared by the inventive methodf-Sb2O3Composite chemical composition is homogeneous, and purity is higher, good crystallinity, and pattern is homogeneous,
Grown on carbon fibers stably the most square phase Sb2O3, this product has been effectively combined carbon fiber and stibium oxide advantage, has had the most simultaneously
Higher specific capacity is had to keep again preferable cycle characteristics.Preparation method of the present invention is simple, and process low temperature is easily-controllable, manufacturing cycle
Short, product good dispersion, environmentally friendly.
Accompanying drawing explanation
Fig. 1 is the C of the embodiment of the present invention 1 preparationf-Sb2O3The XRD figure spectrum of composite.
Fig. 2, Fig. 3 are the C of the embodiment of the present invention 4 preparationf-Sb2O3The SEM photograph of composite.
Fig. 4 is the C of the embodiment of the present invention 6 preparationf-Sb2O3Composite between 0.1～3.0V voltage, 50mAg-1Electric current is close
Under degree, circulate the charge-discharge performance figure of 50 times.
Detailed description of the invention
Below in conjunction with the accompanying drawings and the present invention is described in further detail by embodiment:
Embodiment 1:
1) take the analytically pure CTAB of 0.15g to be dissolved completely in the analytically pure ethanol of 30ml, by 0.85g's in whipping process
SbCl3Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 20 DEG C, and the time is 10h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and oxygen in oven for drying
Change antimony composite.
It can be seen from figure 1 that grown on carbon fibers is the most square phase Sb2O3Powder body, and purity is high, crystallinity is preferable.
Embodiment 2:
1) take the analytically pure CTAB of 0.18g to be dissolved completely in the analytically pure ethanol of 35ml, by 1g's in whipping process
SbCl3Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2.5g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8.5；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 40 DEG C, and the time is 8h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and oxygen in oven for drying
Change antimony composite.
Embodiment 3:
1) take the analytically pure CTAB of 0.16g to be dissolved completely in the analytically pure ethanol of 38ml, by 0.9g's in whipping process
SbCl3Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2.3g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8.8；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 80 DEG C, and the time is 4h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and oxygen in oven for drying
Change antimony composite.
Embodiment 4:
1) take the analytically pure CTAB of 0.2g to be dissolved completely in the analytically pure ethanol of 40ml, by 1.14g's in whipping process
SbCl3Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 3g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8.2；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 100 DEG C, and the time is 2h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and oxygen in oven for drying
Change antimony composite.
From Fig. 2,3 it can be seen that the composite for preparing of embodiment, the Sb of grown on carbon fibers2O3For nanometer wire and
Interlaced reticulating, growth fraction is more uniform, is well combined.
Embodiment 5:
1) take the analytically pure CTAB of 0.19g to be dissolved completely in the analytically pure ethanol of 32ml, by 1.1g's in whipping process
SbCl3Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2.8g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 9；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 50 DEG C, and the time is 6h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and oxygen in oven for drying
Change antimony composite.
Embodiment 6:
1) take the analytically pure CTAB of 0.2g to be dissolved completely in the analytically pure ethanol of 40ml, by 1.14g's in whipping process
SbCl3Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8.5；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 60 DEG C, and the time is 4h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and oxygen in oven for drying
Change antimony composite.
Battery is at 50mAg as seen from Figure 4-1Under electric current density, first discharge specific capacity is 274.17mAhg-1, afterwards
Specific discharge capacity several times constantly declines, and tends to be steady after about 8 times, and final specific discharge capacity is approximately kept at 191mAhg-1Left
Right.
Claims (7)
1. a carbon fiber and the preparation method of stibium oxide composite, it is characterised in that:
1) take the analytically pure CTAB of 0.15-0.2g to be dissolved completely in the analytically pure ethanol of 30-40ml, will in whipping process
The SbCl of 0.85-1.14g3Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2-3g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8～9；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 20 DEG C-100 DEG C, and the time is
2h-10h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and stibium oxide in oven for drying
Composite.
Carbon fiber the most according to claim 1 and the preparation method of stibium oxide composite, it is characterised in that:
1) take the analytically pure CTAB of 0.15g to be dissolved completely in the analytically pure ethanol of 30ml, by the SbCl of 0.85g in whipping process3
Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 20 DEG C, and the time is 10h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and stibium oxide in oven for drying
Composite.
Carbon fiber the most according to claim 1 and the preparation method of stibium oxide composite, it is characterised in that:
1) take the analytically pure CTAB of 0.18g to be dissolved completely in the analytically pure ethanol of 35ml, by the SbCl of 1g in whipping process3Add
To above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2.5g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8.5；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 40 DEG C, and the time is 8h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and stibium oxide in oven for drying
Composite.
Carbon fiber the most according to claim 1 and the preparation method of stibium oxide composite, it is characterised in that:
1) take the analytically pure CTAB of 0.16g to be dissolved completely in the analytically pure ethanol of 38ml, by the SbCl of 0.9g in whipping process3
Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2.3g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8.8；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 80 DEG C, and the time is 4h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and stibium oxide in oven for drying
Composite.
Carbon fiber the most according to claim 1 and the preparation method of stibium oxide composite, it is characterised in that:
1) take the analytically pure CTAB of 0.2g to be dissolved completely in the analytically pure ethanol of 40ml, by the SbCl of 1.14g in whipping process3
Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 3g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8.2；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 100 DEG C, and the time is 2h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and stibium oxide in oven for drying
Composite.
Carbon fiber the most according to claim 1 and the preparation method of stibium oxide composite, it is characterised in that:
1) take the analytically pure CTAB of 0.19g to be dissolved completely in the analytically pure ethanol of 32ml, by the SbCl of 1.1g in whipping process3
Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2.8g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 9；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 50 DEG C, and the time is 6h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and stibium oxide in oven for drying
Composite.
Carbon fiber the most according to claim 1 and the preparation method of stibium oxide composite, it is characterised in that:
1) take the analytically pure CTAB of 0.2g to be dissolved completely in the analytically pure ethanol of 40ml, by the SbCl of 1.14g in whipping process3
Being added to above-mentioned solution, under room temperature, stirring obtains uniform solution A；
2) take in the carbon fiber addition solution A of 2g and be stirred continuously and obtain B solution with ammonia regulation solution PH to 8.5；
3) B solution being placed in temperature control baking oven and carry out solvent thermal reaction and obtain sample, reaction temperature is 60 DEG C, and the time is 4h；
4) samples with water and ethanol are alternately cleaned and sucking filtration is in blocks, then sample is obtained carbon fiber and stibium oxide in oven for drying
Composite.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109768238A (en) * | 2018-12-24 | 2019-05-17 | 肇庆市华师大光电产业研究院 | A kind of Sb-C/S nano-fiber composite material, preparation method and application |
| CN110265643A (en) * | 2019-06-24 | 2019-09-20 | 陕西科技大学 | A kind of Sb2O5The preparation method of/carbon cloth flexibility anode material of lithium-ion battery |
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| CN102167399A (en) * | 2011-05-20 | 2011-08-31 | 浙江大学 | Preparation method of bowknot-shaped antimonous oxide |
| CN102185144A (en) * | 2011-04-02 | 2011-09-14 | 浙江大学 | Metal oxide/graphene composite material and preparation method thereof |
| CN103943837A (en) * | 2014-04-11 | 2014-07-23 | 浙江大学 | Preparation methods of antimony trioxide and antimony trioxide composite material and applications of antimony trioxide and antimony trioxide composite material in sodium-ion batteries |
| US20150333326A1 (en) * | 2014-05-13 | 2015-11-19 | Samsung Electronics Co., Ltd. | Negative electrode active material for non-lithium secondary battery, method of preparing the same, negative electrode for non-lithium secondary battery including the same, and non-lithium secondary battery including the negative electrode |
-
2016
- 2016-09-18 CN CN201610828356.3A patent/CN106252632A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102185144A (en) * | 2011-04-02 | 2011-09-14 | 浙江大学 | Metal oxide/graphene composite material and preparation method thereof |
| CN102167399A (en) * | 2011-05-20 | 2011-08-31 | 浙江大学 | Preparation method of bowknot-shaped antimonous oxide |
| CN103943837A (en) * | 2014-04-11 | 2014-07-23 | 浙江大学 | Preparation methods of antimony trioxide and antimony trioxide composite material and applications of antimony trioxide and antimony trioxide composite material in sodium-ion batteries |
| US20150333326A1 (en) * | 2014-05-13 | 2015-11-19 | Samsung Electronics Co., Ltd. | Negative electrode active material for non-lithium secondary battery, method of preparing the same, negative electrode for non-lithium secondary battery including the same, and non-lithium secondary battery including the negative electrode |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109768238A (en) * | 2018-12-24 | 2019-05-17 | 肇庆市华师大光电产业研究院 | A kind of Sb-C/S nano-fiber composite material, preparation method and application |
| CN109768238B (en) * | 2018-12-24 | 2021-01-15 | 肇庆市华师大光电产业研究院 | Sb-C/S nanofiber composite material, preparation method and application |
| CN110265643A (en) * | 2019-06-24 | 2019-09-20 | 陕西科技大学 | A kind of Sb2O5The preparation method of/carbon cloth flexibility anode material of lithium-ion battery |
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Application publication date: 20161221 |