CN108648922A - The preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material - Google Patents
The preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material Download PDFInfo
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- CN108648922A CN108648922A CN201810364576.4A CN201810364576A CN108648922A CN 108648922 A CN108648922 A CN 108648922A CN 201810364576 A CN201810364576 A CN 201810364576A CN 108648922 A CN108648922 A CN 108648922A
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- carbon fiber
- cotc
- electrode material
- combination electrode
- aluminium hydroxide
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 47
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 36
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 36
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 35
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000007772 electrode material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910021502 aluminium hydroxide Inorganic materials 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 18
- 229910002706 AlOOH Inorganic materials 0.000 claims description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 21
- 229910052786 argon Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000000499 gel Substances 0.000 claims description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000004146 energy storage Methods 0.000 abstract description 2
- 229910000943 NiAl Inorganic materials 0.000 abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 6
- 206010013786 Dry skin Diseases 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 210000002700 urine Anatomy 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
It is by Vacuum-assisted method method to be deposited on substrate both sides with NiAl LDH to prepare using cotton carbon fiber COTC as substrate the invention discloses a kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material；The cotton carbon fiber being prepared/nickel aluminium hydroxide combination electrode material is sandwich structure.The composite material exhibits that the present invention is prepared go out excellent energy-storage property, and specific capacitance value highest can reach 1387Fg‑1.The sandwich structure also has excellent high rate performance.And volume expansion caused by being effectively relieved in charge and discharge process due to free space abundant between NiAl LDH, the composite material have excellent cyclical stability, and stored energy capacitance can keep 96.7% after 5000 charge and discharge cycles.
Description
Technical field
The present invention relates to the preparing technical fields of combination electrode material, and in particular to a kind of cotton carbon fiber, nickel aluminium hydrogen-oxygen
The preparation method of compound combination electrode material.
Background technology
Layered double hydroxide (LDH) is due to unique layer structure, ion interchangeability, at low cost and ring
The characteristics such as border close friend and be widely used in pseudocapacitors electrode material.However in preparation process, LDH lamellas are easy to happen
It stacking, a large amount of active sites is caused to be unable to get utilization, the characteristic of semiconductor of LDH causes it with poor electrical conductance in addition,
It is unfavorable for the progress of faraday's reaction.
In order to solve the above-mentioned technical problem, the prior art carries out LDH and carbon material in relation to research report compound to reach
Optimize LDH nanostructures and improves the purpose of material conductivity.As CN107068416A discloses a kind of carbon material/metal hydrogen-oxygen
The preparation method of compound combination electrode material is ultrasonic disperse after mixing carbon material with water, using dispersion liquid as bottom liquid；So
Double-jet method is used to be respectively delivered to the mixed liquor A configured and mixed liquid B afterwards anti-equipped with bottom liquid with homogenizer
It answers in device and is reacted, later by the way that combination electrode material is made after being detached, washed to reaction product, being dried.
By by carbon material with metal hydroxides is compound makes some progress and improve to prepare electrode material, so
And still have some problem and shortage：Its capacitance is still relatively low, and high rate performance is poor；Structural instability, in charge and discharge process
Easily cause volume expansion, cyclical stability to be improved.
Invention content
In order to solve above-mentioned defect existing in the prior art, present applicant proposes a kind of cotton carbon fiber/nickel aluminium hydrogen-oxygens
The preparation method of compound combination electrode material, using COCT as substrate, NiAl-LDH is deposited on by Vacuum-assisted method method
Substrate both sides, sandwich structure consisting.The cotton carbon fiber that the present invention is prepared/nickel aluminium hydroxide combination electrode material tool
There is excellent cyclical stability.
To achieve the above object, the required main difficult technical overcome is：How cotton carbon fiber and bimetallic are determined
How the preparation process and process conditions of hydroxide control.
Its technical solution includes：
A kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material, is with cotton carbon fiber
COTC is deposited on substrate both sides to prepare as substrate, with NiAl-LDH by Vacuum-assisted method method；The cotton being prepared
Carbon fiber/nickel aluminium hydroxide combination electrode material is sandwich structure.
The advantageous effects that above-mentioned technical proposal is directly brought are：The product purity prepared by Vacuum-assisted method method
Height, good dispersion, stability are strong.Sandwich structure can reinforcing material electric conductivity and high rate performance.
As a preferred solution of the present invention, the preparation process of the cotton carbon fiber is：A certain amount of cotton is taken to tear
It is broken, it is put into baking oven and is dried, take out be placed in tube furnace later, heat under an argon atmosphere, washing is into after natural cooling
Property is drying to obtain；
Argon flow amount is 80mLmin under an argon atmosphere-1, it is heated to 600 DEG C with the heating rate of 5 DEG C/min and keeps
2h。
As another preferred embodiment of the present invention, oven temperature is set as 80 DEG C, 1~3h of drying time.
Further, the Vacuum-assisted method method the specific steps are：
Cotton carbon fiber COTC is distributed in AlOOH gels by a, is passed sequentially through centrifugation, is washed, is dried to obtain
COTC/AlOOH powder；
B, which repeats step a, enables AlOOH to be fully coated on the surfaces COTC as silicon source 3~5 times；
COTC/AlOOH powder obtained by step b is distributed in deionized water by c, and Ni (NO are then added3)2·6H2O and urine
Acquired solution is transferred in reaction kettle in 100 DEG C of crystallization 24 hours by element, stirring；
D pass sequentially through be filtered, washed, dry after up to product.
Further, in step a, cotton carbon fiber COTC and the bulking value proportioning of AlOOH gels are 0.15~0.2:
AlOOH gels described in 30~40g/mL are hydrolyzed by aluminium isopropoxide to be obtained.
Further, repeating step a enables AlOOH to be fully coated on the surfaces COTC as silicon source 4 times.
Further, in step c, the Ni (NO3)2·6H2O and the w/v of deionized water be 0.55~
0.95:The w/v of 40g/mL, the urea and deionized water is 0.4:40g/mL.
Further, washing is neutrality in step d, and drying temperature is 85 DEG C.
Advantageous effects caused by the present invention are：
Cotton carbon fiber has the carbon fiber network of abundant micropore, can effectively be reduced in cotton grown on carbon fibers LDH
The orifice throat length of micropore effectively ensures that material has excellent multiplying power property while introducing a large amount of micropores.
The composite material exhibits that the present invention is prepared go out excellent energy-storage property, and specific capacitance value highest can reach
1387F·g-1.The sandwich structure also has excellent high rate performance.And due to free space abundant between NiAl-LDH
Caused volume expansion in charge and discharge process can be effectively relieved, which has excellent cyclical stability, passes through
Stored energy capacitance can keep 96.7% after 5000 charge and discharge cycles.
Description of the drawings
The present invention will be further described below in conjunction with the accompanying drawings：
Fig. 1 is cotton carbon fiber/nickel aluminum bimetal hydroxide (COTC/ that the embodiment of the present invention 1 is prepared
NiAlOOH stereoscan photograph)；
Fig. 2 is the transmission electricity of 2 cotton carbon fiber of the embodiment of the present invention/nickel aluminum bimetal hydroxide (COTC/NiAlLDH)
Mirror photo.
Specific implementation mode
The present invention proposes a kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material, in order to make
Advantages of the present invention, technical solution are clearer, clear, and with reference to specific embodiment, the present invention will be further described.
Raw material needed for the present invention can be bought by commercial channel and be obtained.
Embodiment 1：
The first step tears up suitable cotton, is put into 100 DEG C of drying 1h of baking oven, the cotton of drying is placed in tubular type later
In stove, (argon flow amount 80mLmin under an argon atmosphere-1), it is heated to 500 DEG C with the heating rate of 5 DEG C/min and keeps
3h.It after natural cooling, is washed to neutrality with hydrochloric acid solution, deionized water, the sample being dried to obtain is denoted as COTC.
Second step, using COCT as substrate, NiAl-LDH is deposited on substrate both sides by Vacuum-assisted method method, composition three
Mingzhi's structure.0.2g COTC are distributed in 40mL AlOOH gels (hydrolyzed and obtained by aluminium isopropoxide) and are stirred first
For 24 hours, by centrifugation, wash, be dried to obtain COTC/AlOOH.Previous step, which is repeated four times, enables AlOOH to be fully coated on
The surfaces COTC are as silicon source.Gained COTC/AlOOH powder is distributed in 60mL deionized waters, 0.85g Ni are then added
(NO3)2·6H2O and 0.40g urea.After stirring 70 minutes, transfer the solution into reaction kettle in 100 DEG C of crystallization 24 hours.It is logical
Product is collected by filtration, it is neutrality to be washed with deionized to filtrate, and gained sample is named as by products obtained therefrom in 85 DEG C of dryings
COTC-NiAlOOH。
The scanning electricity of the cotton carbon fiber that the present embodiment is prepared/nickel aluminum bimetal hydroxide (COTC/NiAlOOH)
Mirror photo is as shown in Figure 1.
Embodiment 2：
The first step tears up suitable cotton, is put into 100 DEG C of drying 1h of baking oven, the cotton of drying is placed in tubular type later
In stove, (argon flow amount 80mLmin under an argon atmosphere-1), it is heated to 500 DEG C with the heating rate of 10 DEG C/min and keeps
3h.It after natural cooling, is washed to neutrality with hydrochloric acid solution, deionized water, the sample being dried to obtain is denoted as COTC.
Second step, using COCT as substrate, NiAl-LDH is deposited on substrate both sides by Vacuum-assisted method method, composition three
Mingzhi's structure.0.2g COTC are distributed in 40mL AlOOH gels (hydrolyzed and obtained by aluminium isopropoxide) and are stirred first
For 24 hours, by centrifugation, wash, be dried to obtain COTC/AlOOH.Previous step, which is repeated four times, enables AlOOH to be fully coated on
The surfaces COTC are as silicon source.Gained COTC/AlOOH powder is distributed in 60mL deionized waters, 0.85g Ni are then added
(NO3)2·6H2O and 0.40g urea.After stirring 70 minutes, transfer the solution into reaction kettle in 100 DEG C of crystallization 24 hours.It is logical
Product is collected by filtration, it is neutrality to be washed with deionized to filtrate, and gained sample is named as by products obtained therefrom in 85 DEG C of dryings
COTC-NiAlOOH。
The transmission electron microscope photo of the present embodiment cotton carbon fiber/nickel aluminum bimetal hydroxide (COTC/NiAlLDH) is as schemed
Shown in 2.
Embodiment 3：
The first step tears up suitable cotton, is put into 100 DEG C of drying 1h of baking oven, the cotton of drying is placed in tubular type later
In stove, (argon flow amount 80mLmin under an argon atmosphere-1), it is heated to 500 DEG C with the heating rate of 5 DEG C/min and keeps
3h.It after natural cooling, is washed to neutrality with hydrochloric acid solution, deionized water, the sample being dried to obtain is denoted as COTC.
Second step, using COCT as substrate, NiAl-LDH is deposited on substrate both sides by Vacuum-assisted method method, composition three
Mingzhi's structure.0.2g COTC are distributed in 40mL AlOOH gels (hydrolyzed and obtained by aluminium isopropoxide) and are stirred first
For 24 hours, by centrifugation, wash, be dried to obtain COTC/AlOOH.AlOOH is set fully to be coated in triplicate previous step
The surfaces COTC are as silicon source.Gained COTC/AlOOH powder is distributed in 40mL deionized waters, 0.55g Ni are then added
(NO3)2·6H2O and 0.40g urea.After stirring 70 minutes, transfer the solution into reaction kettle in 100 DEG C of crystallization 24 hours.It is logical
Product is collected by filtration, it is neutrality to be washed with deionized to filtrate, and gained sample is named as by products obtained therefrom in 85 DEG C of dryings
COTC-NiAlOOH。
Embodiment 4：
The first step tears up suitable cotton, is put into 100 DEG C of drying 1h of baking oven, the cotton of drying is placed in tubular type later
In stove, (argon flow amount 80mLmin under an argon atmosphere-1), it is heated to 500 DEG C with the heating rate of 5 DEG C/min and keeps
3h.It after natural cooling, is washed to neutrality with hydrochloric acid solution, deionized water, the sample being dried to obtain is denoted as COTC.
Second step, using COCT as substrate, NiAl-LDH is deposited on substrate both sides by Vacuum-assisted method method, composition three
Mingzhi's structure.0.2g COTC are distributed in 40mL AlOOH gels (hydrolyzed and obtained by aluminium isopropoxide) and are stirred first
For 24 hours, by centrifugation, wash, be dried to obtain COTC/AlOOH.Previous step, which is repeated five times, enables AlOOH to be fully coated on
The surfaces COTC are as silicon source.Gained COTC/AlOOH powder is distributed in 40mL deionized waters, 0.9 5g Ni are then added
(NO3)2·6H2O and 0.40g urea.After stirring 70 minutes, transfer the solution into reaction kettle in 100 DEG C of crystallization 24 hours.It is logical
Product is collected by filtration, it is neutrality to be washed with deionized to filtrate, and gained sample is named as by products obtained therefrom in 85 DEG C of dryings
COTC-NiAlOOH。
Embodiment 5：
The first step tears up suitable cotton, is put into 100 DEG C of drying 1h of baking oven, the cotton of drying is placed in tubular type later
In stove, (argon flow amount 80mLmin under an argon atmosphere-1), it is heated to 500 DEG C with the heating rate of 5 DEG C/min and keeps
3h.It after natural cooling, is washed to neutrality with hydrochloric acid solution, deionized water, the sample being dried to obtain is denoted as COTC.
Second step, using COCT as substrate, NiAl-LDH is deposited on substrate side by Vacuum-assisted method method.First will
0.2g COTC are distributed in 40mL AlOOH gels (hydrolyzed and obtained by aluminium isopropoxide) and stir for 24 hours, by centrifuging,
It washs, be dried to obtain COTC/AlOOH.Previous step, which is repeated four times, enables AlOOH to be fully coated on the surfaces COTC as silicon source.
Gained COTC/AlOOH powder is distributed in 60mL deionized waters, 0.85g Ni (NO are then added3)2·6H2O and 0.40g urine
Element.After stirring 70 minutes, transfer the solution into reaction kettle in 100 DEG C of crystallization 24 hours.Product is collected by filtration, spend from
Sub- water washing to filtrate is neutrality, and products obtained therefrom is named as COTC-NiAlOOH in 85 DEG C of dryings, by gained sample.To the present invention
The COTC-NiAlOOH that embodiment 1- embodiments 5 are prepared makees following analysis detection, and testing result is as shown in table 1.
Table 1
Under above-described embodiment 1 to the guide of embodiment 5, other unrequited combination those skilled in the art
It is obvious to realize.
It should be noted that any equivalent way that those skilled in the art are made under the introduction of this specification, or
Obvious variant should all be within the scope of the present invention.
Claims (8)
1. a kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material, it is characterised in that：It is with cotton
Carbon fiber COTC is deposited on substrate both sides to prepare as substrate, with NiAl-LDH by Vacuum-assisted method method；It is prepared
Cotton carbon fiber/nickel aluminium hydroxide combination electrode material be sandwich structure.
2. a kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material according to claim 1,
It is characterized in that, the preparation process of the cotton carbon fiber is：It takes a certain amount of cotton to tear up, is put into baking oven and is dried, later
Taking-up is placed in tube furnace, is heated under an argon atmosphere, is washed after natural cooling to neutrality, is drying to obtain；
Argon flow amount is 80mLmin under an argon atmosphere-1, it is heated to 600 DEG C with the heating rate of 5 DEG C/min and keeps 2h.
3. a kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material according to claim 2,
It is characterized in that：Oven temperature is set as 80 DEG C, 1~3h of drying time.
4. a kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material according to claim 1,
Be characterized in that, the Vacuum-assisted method method the specific steps are：
Cotton carbon fiber COTC is distributed in AlOOH gels by a, is passed sequentially through centrifugation, is washed, is dried to obtain COTC/
AlOOH powder；
B, which repeats step a, enables AlOOH to be fully coated on the surfaces COTC as silicon source 3~5 times；
COTC/AlOOH powder obtained by step b is distributed in deionized water by c, and Ni (NO are then added3)2·6H2O and urea, are stirred
It mixes, acquired solution is transferred in reaction kettle in 100 DEG C of crystallization 24 hours；
D pass sequentially through be filtered, washed, dry after up to product.
5. a kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material according to claim 4,
It is characterized in that：In step a, cotton carbon fiber COTC and the bulking value proportioning of AlOOH gels are 0.15~0.2:30~40g/
ML, the AlOOH gels are hydrolyzed by aluminium isopropoxide and are obtained.
6. a kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material according to claim 4,
It is characterized in that：Repeating step a enables AlOOH to be fully coated on the surfaces COTC as silicon source 4 times.
7. a kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material according to claim 4,
It is characterized in that：In step c, the Ni (NO3)2·6H2O and the w/v of deionized water are 0.55~0.95:40g/
The w/v of mL, the urea and deionized water is 0.4:40g/mL.
8. a kind of preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material according to claim 4,
It is characterized in that：Washing is neutrality in step d, and drying temperature is 85 DEG C.
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| CN201810364576.4A CN108648922A (en) | 2018-04-23 | 2018-04-23 | The preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material |
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2018
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