CN110289179A - Reactive metal oxides-carbonization bacteria cellulose electrode material preparation method - Google Patents
Reactive metal oxides-carbonization bacteria cellulose electrode material preparation method Download PDFInfo
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- CN110289179A CN110289179A CN201910456924.5A CN201910456924A CN110289179A CN 110289179 A CN110289179 A CN 110289179A CN 201910456924 A CN201910456924 A CN 201910456924A CN 110289179 A CN110289179 A CN 110289179A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/40—Fibres
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of reactive metal oxides-carbonization bacteria cellulose electrode material preparation methods.The method first uses electrochemical oxidation process to carry out surface hydrophilic processing to carbonization bacteria cellulose, then the ethanol solution of active metal nitrate is impregnated, after the ethyl alcohol volatilization in material, it is passed through ammonia in nitrate-carbonization bacteria cellulose film, obtains reactive metal oxides-carbonization bacteria cellulose film composite material of light flexible through gas precipitation.In composite material produced by the present invention, nickel oxide dispersibility with higher can inhibit reunion of the nickel oxide isoreactivity material in carbonization bacterial cellulose three-dimensional structure, be suitable for supercapacitor field.
Description
Technical field
The invention belongs to the preparation technical fields of composite material, are related to a kind of reactive metal oxides-carbonization bacterial fibers
The preparation method of plain electrode material.
Background technique
Bacteria cellulose is the natural fiber generated by fermentation process, compared with artificial synthetic fiber element, tool
Have many excellent physics and chemistry and mechanical performance, as biodegradability, good three-dimensional net structure, higher chemical purity and
Preferable mechanical strength etc., is generally used for the industries such as electrochemistry, medicine and food.The synthesis of bacteria cellulose only needs inexpensively
Raw material, such as glucose, sucrose and abandoned biomass acid hydrolysis solution, and these raw material are renewable resources, and micro- life
Object combined coefficient is a kind of preparation method of green, has become the research hotspot of novel biomaterial much higher than artificial synthesized.
Bacteria cellulose nanofiber is formed three-dimensional netted with relatively uniform micrometer level porous structure, and three-dimensional space effect can
To promote substance high efficiency of transmission wherein.The dimensional effect of nanofiber can provide active site for the deposition of many substances,
Many effective nano active substances can be loaded in fiber surface.
Doing bacteria cellulose with the compound of metal oxide active substance at present is to carry out in the solution mostly, active material
Morphology and size be more difficult to get effective control, the energy density and power density of composite material obtained are lower.Lu Min et al.
Using the blending precipitation method in bacteria cellulose area load Fe3O4Particle, and be applied in the absorption of heavy metal cadmium ion (Lu Min,
Guan Xiaohui, Wei Dezhou bacterial cellulose loaded nanometer Fe3O4Preparation and its absorption Cd2+Research [J] safety and environmentology
Report, 2011,11 (5): 22-25.).Lei Jia et al. utilizes in situ synthesis, and nanogold is compound with bacteria cellulose, and tests
Its catalytic performance.But in the composite material of above method preparation, metallic particles is easy to reunite, and size inhomogenous (Lei Jia, Qiu
Its power, Jiang Weiyan bacteria cellulose/nanogold laminated film original position controllable preparation and catalytic performance study [J] non-ferrous metal:
Smelting Part, 2016 (9): 42-47.).
Summary of the invention
For in the prior art carbonization bacteria cellulose in situ deposited metal activating oxide when, active material is in three-dimensional
Easy to reunite in space structure, thus the problems such as inhibiting the electro-chemical activity of composite material, the present invention provides a kind of active metal oxygen
Compound-carbonization bacteria cellulose electrode material preparation method.
Technical scheme is as follows:
Reactive metal oxides-carbonization bacteria cellulose electrode material preparation method is led to using bacteria cellulose as raw material
The three-dimensional structure for crossing the preparatory anchoring fiber element of high-temperature calcination obtains the carbonization bacteria cellulose of light flexible, then uses constant potential
Method does surface hydrophilic processing, impregnates metal oxide precursor solution, oxidizes metal object presoma equably after solvent flashing
It is distributed in fiber surface, is finally passed through gas into fibre three-dimensional network structure, metal oxide is realized using gas precipitation agent
For presoma to the efficient transition of metal oxide, carbonization bacteria cellulose metal oxides, which are made, has the compound of polymolecularity
Material, specifically includes the following steps:
Step 1, using constant potential anodizing to carbonization bacteria cellulose carry out surface oxidation, oxidizing potential be 2~
5V, oxidization time are 100~300s, obtain hydrophilic flexible carbonization bacteria cellulose；
Step 2, hydrophilic flexible carbonization bacteria cellulose is immersed in the ethanol solution of active metal nitrate, is soaked
After finishing entirely, ethyl alcohol is removed, active metal nitrate-carbonization bacteria cellulose is obtained；
Step 3, using gas precipitation method, ammonium hydroxide is heated, the ammonia of generation is fine through active metal nitrate-carbonization bacterium
Dimension element, the active metal nitrate reaction with carbonization bacteria cellulose fibre surface, obtains reactive metal oxides-carbon flexible
Change bacteria cellulose electrode material.
Preferably, in step 1, the carbonization bacteria cellulose is prepared using static culture and high-temperature calcination, specially
The bacteria cellulose film that static culture is obtained is placed in calcine at 700~1000 DEG C and be made.
Preferably, in step 2, the soaking time is 1~2h.
Preferably, in step 2, the active metal is nickel, iron, manganese or cobalt.
Preferably, in step 2, the concentration of the ethanol solution of the active metal nitrate is 0.02~0.1M.
In step 3, the metal nitrate is to the conversion of metal oxide using ammonia as gas precipitation agent, gas
The temperature of precipitation system is 110~130 DEG C.
Compared with prior art, the invention has the following advantages that
(1) carbonization bacteria cellulose is that the natural fiber generated by fermentation process is carbonized, diameter ruler
It is very little to be less than 100nm, belong to nano-scale fiber, size is only the 1/10 of artificial synthetic fiber, the three dimensional network that nanofiber is formed
Shape has relatively uniform micrometer level porous structure, and three-dimensional space effect can promote substance high efficiency of transmission wherein, Nanowire
The dimensional effect of dimension can provide active site for the deposition of many substances, fix three-dimensional structure by high-temperature calcination, can be
Nano active substance is provided convenience in fiber surface load；
(2) hydrophilic treated, modified hydrophily are made to carbonization bacteria cellulose surface using constant potential anodizing
Carbonization bacteria cellulose provides preferable active site for the attachment of metal oxide precursor；
(3) reactive metal oxides-carbonization bacteria cellulose using the preparation of ammonia oxidation activity metal nitrate is compound
Material has many advantages, such as light flexible, metal oxide dispersibility with higher, and composite material ability with higher is close
Degree is suitable for the fields such as supercapacitor.
Detailed description of the invention
Fig. 1 is reactive metal oxides of the invention-carbonization bacteria cellulose electrode material preparation flow figure.
Fig. 2 is the flexible display diagram of carbonization bacteria cellulose.
Fig. 3 is nickel oxide-carbonization bacteria cellulose XPS map (a), the narrow spectrum (b) of Ni element, the narrow spectrum of carbon
(c) and the narrow spectrum (d) of oxygen element.
Fig. 4 is nickel oxide-carbonization bacteria cellulose transmission electron microscope figure.
Fig. 5 is carbonization bacteria cellulose and nickel oxide-carbonization bacteria cellulose charging and discharging curve under conditions of 0.2A/g
Figure.
Fig. 6 is embodiment 1 (a), nickel oxide-carbonization bacterial fibers obtained made from comparative example 1 (b) and comparative example 2 (c)
The SEM of plain composite material schemes.
Specific embodiment
The present invention is further described in detail below with reference to embodiment and attached drawing.
The following carbonization bacteria celluloses used in the examples of the present invention, are prepared by following steps: by glucose, phosphoric acid
Disodium hydrogen, citric acid, yeast extract, peptone are added to the water, and dissolve, are uniformly mixed adjusting pH to 6.0, wet process is gone out at 121 DEG C
Bacterium 30min, with 10% inoculum concentration access seed liquor, culture 48h obtain the thick film of bacteria cellulose, in 85 DEG C 0.3% hydrogen
It after heating 2h in sodium hydroxide solution, is cleaned with deionized water to neutrality, obtains bacteria cellulose film, be lyophilized spare.Bacterial fibers
The high-temperature calcination at 700~1000 DEG C in inert atmosphere of plain film obtains carbonization bacteria cellulose flexible.
Embodiment 1
Step 1, using constant potential anodizing to carbonization bacteria cellulose fibre surface oxidation, oxidizing potential and oxidation
Time is respectively 2V and 300s, obtains hydrophilic flexible carbonization bacteria cellulose material.
Step 2, hydrophilic flexible carbonization bacteria cellulose material is immersed in 2h in 0.02M nickel nitrate solution, then
Ethyl alcohol is volatilized under the conditions of 60 DEG C, obtains nickel nitrate-carbonization bacteria cellulose material.
Step 3, nickel nitrate flexible-carbonization bacteria cellulose membrane material is covered in closed ammonium hydroxide beaker, 110
Make ammonia through nickel nitrate-carbonization bacteria cellulose film, the nitric acid of ammonia and carbonization bacteria cellulose fibre surface under the conditions of DEG C
Nickel reactant obtains nickel oxide flexible-carbonization bacteria cellulose material.
Embodiment 2
Step 1, using constant potential anodizing to carbonization bacteria cellulose fibre surface oxidation, oxidizing potential and oxidation
Time is respectively 5V and 100s, obtains hydrophilic flexible carbonization bacteria cellulose material.
Step 2, hydrophilic flexible carbonization bacteria cellulose material is immersed in 0.05M nickel nitrate solution, 1h, then
Ethyl alcohol is volatilized under the conditions of 60 DEG C, obtains nickel nitrate-carbonization bacteria cellulose material.
Step 3, nickel nitrate flexible-carbonization bacteria cellulose membrane material is covered in closed ammonium hydroxide beaker, 120
Make ammonia through nickel nitrate-carbonization bacteria cellulose film, the nitric acid of ammonia and carbonization bacteria cellulose fibre surface under the conditions of DEG C
Nickel reactant obtains nickel oxide flexible-carbonization bacteria cellulose material.
Embodiment 3
Step 1, using constant potential anodizing to carbonization bacteria cellulose fibre surface oxidation, oxidizing potential and oxidation
Time is respectively 5V and 300s, obtains hydrophilic flexible carbonization bacteria cellulose material.
Step 2, hydrophilic flexible carbonization bacteria cellulose material is immersed in 1h in 0.1M nickel nitrate solution, then existed
Ethyl alcohol is volatilized under the conditions of 60 DEG C, obtains nickel nitrate-carbonization bacteria cellulose material.
Step 3, nickel nitrate flexible-carbonization bacteria cellulose membrane material is covered in closed ammonium hydroxide beaker, 130
Make ammonia through nickel nitrate-carbonization bacteria cellulose film, the nitric acid of ammonia and carbonization bacteria cellulose fibre surface under the conditions of DEG C
Nickel reactant obtains nickel oxide flexible-carbonization bacteria cellulose material.
Embodiment 4
Step 1, using constant potential anodizing to carbonization bacteria cellulose fibre surface oxidation, oxidizing potential and oxidation
Time is respectively 5V and 300s, obtains hydrophilic flexible carbonization bacteria cellulose material.
Step 2, it prepares, hydrophilic flexible carbonization bacteria cellulose material is immersed in the nickel nitrate solution of 0.1M concentration
Then middle 2h volatilizees ethyl alcohol under the conditions of 60 DEG C, obtain nitrate-carbonization bacteria cellulose material.
Step 3, nickel nitrate flexible-carbonization bacteria cellulose membrane material is covered in closed ammonium hydroxide beaker, 130
Make ammonia through nickel nitrate-carbonization bacteria cellulose film, the nitric acid of ammonia and carbonization bacteria cellulose fibre surface under the conditions of DEG C
Nickel reactant obtains nickel oxide flexible-carbonization bacteria cellulose material.
Nickel oxide made from each embodiment-carbonization bacteria cellulose material as shown in Fig. 2, carbonization bacteria cellulose have compared with
Good flexibility.The XPS elemental analysis of the nickel oxide that each embodiment obtains-carbonization composite material as shown in figure 3,
Contain C, O, Ni and micro N element in compound as the result is shown, wherein the peak O=C-O in C element from electrochemical oxidation,
The peak Ni2p of nickel element and the nickel element base peak for analyzing pure NiO almost coincide.Nickel oxide obtained-carbonization bacterial fibers
The transmission electron microscope figure of plain compound is as shown in figure 4, metal oxide is uniformly dispersed in the surface of fiber.Carbon obtained
Change bacteria cellulose and nickel oxide-carbonization composite material is assembled into the charging and discharging curve such as figure that supercapacitor measures
Shown in 5, the charge/discharge curve for the bacteria cellulose that is carbonized is more symmetrical, and at linear triangle, this shows that it has height can
Inverse electrochemical behavior.And nickel oxide-carbonization composite material charge/discharge curve is more asymmetric, shows to aoxidize
Nickel has preferable energy-storage property, and the charge/discharge capacity of compound is 307.1mAh, and the charge and discharge for the bacteria cellulose that is carbonized
Capacity is 100.9mAh, illustrates that the charge/discharge capacity of compound is higher.
Comparative example 1
This comparative example is substantially the same manner as Example 1, it is unique unlike constant potential anodizing without step 1.
The SEM figure for the material being prepared is as shown in Fig. 6 (b).
Comparative example 2
This comparative example is different from embodiment, and first bacteria cellulose film is immersed in ethanolic nitrate solution, after freeze-drying, then
The high-temperature calcination at 800 DEG C, is prepared into metal-carbide oxide-bacteria cellulose electrode material, and SEM schemes such as Fig. 6 (c) institute
Show.
(a) is the SEM figure (embodiment) for carrying out constant potential anodic oxidation operation preparation obtained electrode material in Fig. 6；(b)
(comparative example 1) is schemed for the SEM for the electrode material being prepared without constant potential anodic oxidation；It (c) is advanced row metal nitric acid
Salt impregnates the SEM figure (comparative example 2) for carrying out the electrode material that freeze-drying carbonization is prepared again.It can be seen from the figure that using this
The electrode material that the method for invention is prepared is able to maintain that tridimensional network, and uniformly loads metal oxygen in the fibre
Compound particle, and do not use constant potential anodic oxidation operation preparation electrode material, due to be carbonized bacteria cellulose surface hydrophobicity,
It is carried on carbonization bacteria cellulose almost without metallic particles, carbonization system is lyophilized again using direct metal-nitrate solutions of impregnating
Standby electrode material, due to the entrance of metal ion, the three-dimensional structure of bacteria cellulose has just been collapsed when freeze-drying, and metal
The agglomeration of ion is obvious.
Claims (7)
1. reactive metal oxides-carbonization bacteria cellulose electrode material preparation method, which is characterized in that including following step
It is rapid:
Step 1, surface oxidation is carried out to carbonization bacteria cellulose using constant potential anodizing, oxidizing potential is 2~5V, oxygen
The change time is 100~300s, obtains hydrophilic flexible carbonization bacteria cellulose；
Step 2, hydrophilic flexible carbonization bacteria cellulose is immersed in the ethanol solution of active metal nitrate, has been impregnated
Quan Hou removes ethyl alcohol, obtains active metal nitrate-carbonization bacteria cellulose；
Step 3, using gas precipitation method, ammonium hydroxide is heated, the ammonia of generation penetrates active metal nitrate-carbonization bacterial fibers
Element, the active metal nitrate reaction with carbonization bacteria cellulose fibre surface, obtains reactive metal oxides-carbonization flexible
Bacteria cellulose electrode material.
2. preparation method according to claim 1, which is characterized in that in step 1, the carbonization bacteria cellulose is used
Static culture and high-temperature calcination preparation.
3. preparation method according to claim 1 or 2, which is characterized in that in step 1, the carbonization bacteria cellulose
It is placed in calcine at 700~1000 DEG C by the bacteria cellulose film for obtaining static culture and be made.
4. preparation method according to claim 1, which is characterized in that in step 2, the soaking time is 1~2h.
5. preparation method according to claim 1, which is characterized in that in step 2, the active metal is nickel, iron, manganese
Or cobalt.
6. preparation method according to claim 1, which is characterized in that in step 2, the second of the active metal nitrate
The concentration of alcoholic solution is 0.02~0.1M.
7. preparation method according to claim 1, which is characterized in that in step 3, the metal nitrate is to metal oxygen
Using ammonia as gas precipitation agent, the temperature of gas precipitation system is 110~130 DEG C for the conversion of compound.
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| CN111210997A (en) * | 2020-02-13 | 2020-05-29 | 海南师范大学 | Novel MnOmPreparation method and application of @ BCCNFs composite material |
| CN113600146A (en) * | 2021-07-26 | 2021-11-05 | 武汉大学 | Iron-manganese composite membrane adsorbent, preparation method thereof and application thereof in adsorbing arsenic and cadmium in water and soil |
| CN113600146B (en) * | 2021-07-26 | 2022-07-29 | 武汉大学 | Iron-manganese composite membrane adsorbent, preparation method thereof and application thereof in adsorbing arsenic and cadmium in water and soil |
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