CN106057486A - Carbon sphere-Fe oxide composite material and preparation method and use thereof - Google Patents
Carbon sphere-Fe oxide composite material and preparation method and use thereof Download PDFInfo
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- CN106057486A CN106057486A CN201610312374.6A CN201610312374A CN106057486A CN 106057486 A CN106057486 A CN 106057486A CN 201610312374 A CN201610312374 A CN 201610312374A CN 106057486 A CN106057486 A CN 106057486A
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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
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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
- H01G11/46—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 present invention relates to a preparation method of a carbon sphere-Fe oxide composite material. The method comprises the following steps of S1 reacting dried waxberries, deionized water and Fe compounds in a high-pressure reactor; S2 after the reaction is ended, releasing the pressure to a normal pressure, naturally cooling to a room temperature, and washing, vacuuming and drying the obtained solid to obtain a dried sample; S3 carrying out the high-temperature processing on the dried sample under the protection of an inert gas to obtain the carbon sphere-Fe oxide composite material. The carbon sphere-Fe oxide composite material has an excellent electrical property, so that the carbon sphere-Fe oxide composite material can be applied to the capacitor field, in particular to the super capacitor field, and has the good application prospect and industrialization potential.
Description
Technical field
The invention provides a kind of composite and preparation method thereof and purposes, more specifically, it is provided that a kind of available
Carbon ball-iron composite material in super capacitor material and preparation method thereof and purposes, belong to inorganic functional material and electrochemistry
Energy technology field.
Background technology
Ultracapacitor, as a kind of novel clean energy technology, is a kind of novel, efficient, practical energy storage dress
Put, there is the superior performances such as Large Copacity, high power, long-life, with low cost, environmental friendliness, be the one of energy storage field
Item revolutionary development, and traditional storage battery can be replaced in some field, play the advantage that battery can not play.
But, at present the electrode material with activated carbon as ultracapacitor there is also high current charge-discharge difficulty, energy close
Spend the defects such as on the low side, cycle life is short, this greatly limits large-scale application and the industrialization of ultracapacitor.
Therefore, the CNT of material with carbon element such as one-dimentional structure of new structure or carbon nano-fiber, two-dimensional structure are found
Graphene, the porous carbon etc. of three-dimensional multistage structure become current study hotspot.Although these new materials can carry effectively
Its performance high, but still suffer from many defects such as this cost is high, building-up process is complicated, the reality that can not meet ultracapacitor should
With requiring.
At present, discarded biomass cause vast research work with its low cost, the excellent characteristics such as renewable, pollution-free
The concern of person, such as:
Peng et al. utilizes five kinds of useless Folium Camelliae sinensis from China, first through high temperature carbonization, then activates with KOH, is had
There are loose structure, high-specific surface area (2245-2841m2/ g) material with carbon element, this material shows preferable capacitance behavior:
When electric current density is 1A/g, it is up to 330F/g than electric capacity；Additionally, the electric capacity after 2000 circulations is still initial capacity
92%.
Li et al. utilizes Fructus Solani melongenae for raw material, and Fructus Solani melongenae obtains after lyophilization the carbon material of the laminated structure of a kind of porous
Material, when sweep speed is 5mv/s, capacitance is up to 121F/g, when electric current density is 10A/g, electric capacity after circulation 10000 circle
Conservation rate has 92%.
Cheng et al. utilizes mushroom for raw material, obtains the material with carbon element of a kind of grading-hole, when electric current density is 3A/g, and circulation
After 15000 circles, capacity retention has 95.7%.
As it has been described above, prior art discloses the multiple method utilizing abandoned biomass to prepare new material, and thus
Obtain the multiple new material with excellent electrical properties, although but these new materials can be by biomass through direct carbon
Change, activation and be provided with the performance such as porous, high-specific surface area, but on electric property, still suffer from that high current charge-discharge is poor, energy
The defects such as metric density is relatively low, this severely limits application and the industrialized production of its reality.
Therefore, based on preparing the defect of electrode material for super capacitor currently with biomass, new method how is utilized to carry
High its performance tool is of great significance, and is also study hotspot and the emphasis of current electrochemical energy source domain, and this is the most just
Basic place and power that the present invention is accomplished are leaned on.
Summary of the invention
In order to research and develop novel electricity material, especially obtain can be used for the composite in ultracapacitor field, this
A person of good sense conducts in-depth research, and after having paid substantial amounts of creative work, thus completes the present invention.
Specifically, technical scheme and content relate to carbon ball-silicon/iron oxide composite material and preparation method thereof
With purposes.
More particularly it relates to following many aspects.
First aspect, the present invention relates to the preparation method of a kind of carbon ball-silicon/iron oxide composite material, and described method includes
Following steps:
S1: Fructus Myricae rubrae is dry, deionized water and iron compound react in high-pressure reactor；
S2: after reaction terminates, pressure release is to normal pressure, and naturally cools to room temperature, washs gained solid, is vacuum dried,
To drying sample；
S3: described drying sample is carried out under inert gas shielding high-temperature process, thus obtains described carbon ball-ferrum oxidation
Thing composite.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step sl, described Fructus Myricae rubrae does
Being fresh Waxberry enucleation the abundant Fructus Myricae rubrae obtained after drying to be done, such as its biodiversity content is less than 10%.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step sl, described ferrum chemical combination
Thing is any one or the most multiple mixture, most preferably iron sulfate in ferric nitrate, iron sulfate or iron chloride.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step sl, Fructus Myricae rubrae dry with
The mass ratio of iron compound is 5-20:1, such as, can be 5:1,10:1,15:1 or 20:1, most preferably 10:1.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step sl, Fructus Myricae rubrae does and goes
The mass ratio of ionized water is 1:1-3, such as, can be 1:1,1:2 or 1:3.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step sl, reaction pressure is
1-5MPa, the reaction pressure of the most described high-pressure reactor is 1-5MPa, such as, can be 1MPa, 2MPa, 3MPa, 4MPa or 5MPa.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step sl, reaction temperature is
160-220 DEG C, such as, can be 160 DEG C, 180 DEG C, 200 DEG C or 220 DEG C.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step sl, the response time is
20-28 hour, such as, can be 20 hours, 22 hours, 24 hours, 26 hours or 28 hours.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step s 2, gained solid can
Being washed with deionized, washing times can be 2-4 time.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step s 2, vacuum drying temperature
Degree for 60-100 DEG C, such as, can be 60 DEG C, 80 DEG C or 100 DEG C；Drying time is 8-12 hour, such as, can be 8 hours, 10 hours
Or 12 hours.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step s3, at described high temperature
The temperature of reason is 800-1000 DEG C, such as, can be 800 DEG C, 850 DEG C, 900 DEG C, 950 DEG C or 1000 DEG C, preferably 850-950 DEG C,
Most preferably 900 DEG C.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step s3, during high-temperature process
Between be 1-3 hour, can be such as 1 hour, 2 hours or 3 hours.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, in step s3, described indifferent gas
Body is nitrogen or argon.
In the preparation method of the described carbon ball-silicon/iron oxide composite material of the present invention, at the high temperature in described step 3
Reason, will place 1-3 hour with atmosphere of inert gases under said temperature scope by described drying sample, thus obtains the present invention
Described carbon ball-silicon/iron oxide composite material.
The inventors discovered that, when above-mentioned preparation method some optimizing technology parameters the most therein using the present invention
Time, it is possible to obtain the carbon ball-silicon/iron oxide composite material with superior electrical performance, and when changing some technological parameter, all
Performance is caused to significantly reduce.
Second aspect, the present invention relates to the carbon ball-silicon/iron oxide composite material obtained by above-mentioned preparation method.
The inventors discovered that, described carbon ball-silicon/iron oxide composite material has the electric property of excellence, thus can be applicable to
Capacitor area, especially ultracapacitor field, have a good application prospect and industrialization potential.
Therefore, the 3rd aspect, the present invention relates to described carbon ball-silicon/iron oxide composite material use in preparing capacitor
On the way.
In the described purposes of the present invention, described carbon ball-silicon/iron oxide composite material can be used to prepare electrode for capacitors.
The preparation method of described electrode for capacitors specifically includes following steps:
(A) weigh the composite of the present invention, acetylene black, PTFE (politef) emulsion (three's mass ratio is 80:
10:10), add ethanol in proper amount, mix homogeneously, when being stirred continuously into starchiness, be coated onto in nickel foam；
(B) nickel foam coating described composite is dried, dries, tabletting, i.e. obtain described electrode for capacitors.
4th aspect, the present invention relates to a kind of electrode for capacitors comprising described carbon ball-silicon/iron oxide composite material, especially
It is electrode of super capacitor.
Inventor is found by research, and the electrode for capacitors comprising described carbon ball-silicon/iron oxide composite material has well
Chemical property, the superior performance such as such as Large Copacity, high power, long-life, with low cost, environmental friendliness, thus can answer
For capacitor especially ultracapacitor field.
As it has been described above, the invention provides a kind of carbon ball-silicon/iron oxide composite material and its production and use, described
Carbon ball-silicon/iron oxide composite material has the electric property of excellence, can be used to prepare electrode for capacitors especially ultracapacitor
Electrode, thus can be used in capacitor especially ultracapacitor, at electricity field, there is huge application potential and industry valency
Value.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture (TEM) of the carbon ball-silicon/iron oxide composite material of the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of the carbon ball-silicon/iron oxide composite material obtained by the embodiment of the present invention 1.
Fig. 3 is the XPS figure of the carbon ball-silicon/iron oxide composite material obtained by the embodiment of the present invention 1.
Fig. 4 is the ferrum high-resolution XPS figure of the carbon ball-silicon/iron oxide composite material obtained by the embodiment of the present invention 1.
Fig. 5 be use the carbon ball-silicon/iron oxide composite material of the embodiment of the present invention 1 and prepared electrode for capacitors in difference
Cyclic voltammogram under sweep speed.
Fig. 6 be use the carbon ball-silicon/iron oxide composite material of the embodiment of the present invention 1 and prepared electrode for capacitors in difference
Constant current charge-discharge figure under electric current density.
Fig. 7 is the big electricity using the carbon ball-silicon/iron oxide composite material of the embodiment of the present invention 1 and prepared electrode for capacitors
Stream charge-discharge performance figure.
Fig. 8 is to use the carbon ball-silicon/iron oxide composite material of the embodiment of the present invention 1 and prepared electrode for capacitors
Ragone schemes.
Fig. 9 be use the carbon ball-silicon/iron oxide composite material of the embodiment of the present invention 1 and prepared electrode for capacitors at 80A/
Cyclical stability figure under g electric current density.
Figure 10 is to use the composite of embodiment of the present invention 1-3 respectively and the constant current charge-discharge of prepared electrode for capacitors
Figure.
The scanning electron microscope (SEM) photograph (SEM) of the composite of the embodiment 4 when Figure 11 is to be not added with iron compound.
Figure 12 is to use the embodiment of the present invention 1, the composite of 4-6 and prepared electrode for capacitors at 1000mv/s respectively
Sweep speed under cyclic voltammogram.
Figure 13 is to use the embodiment of the present invention 1, the composite of 7-8 and prepared electrode for capacitors at 1000mv/s respectively
Sweep speed under cyclic voltammogram.
Detailed description of the invention
Below by concrete drawings and Examples, the present invention is described in detail, but these exemplary accompanying drawing and enforcements
The purposes of mode and purpose are only used for enumerating the present invention, not constitute any type of any to the real protection scope of the present invention
Limit, more non-protection scope of the present invention is confined to this.
Embodiment 1
(i.e. Fructus Myricae rubrae does and iron compound for S1: fully dry 100g Fructus Myricae rubrae is dry, 200g deionized water and 10g iron sulfate
Mass ratio be 10:1) react in the high-pressure reactor of 3MPa, reaction temperature is 200 DEG C, and the response time is 24 hours；
S2: after reaction terminates, pressure release is to normal pressure, and naturally cools to room temperature, is fully washed by gained solid deionized water
Wash 2-4 time, be vacuum dried 10 hours at 80 DEG C, obtain drying sample；
S3: described drying sample is carried out under argon shield high-temperature process, thus obtains carbon ball-iron oxides composite wood
Material, by its named CL1；The temperature of wherein said high-temperature process is 900 DEG C, the process time is 2 hours.
Embodiment 2-3: the investigation of high-temperature process temperature in step S3
In addition to the high-temperature process temperature in step S3 is replaced with 800 DEG C and 1000 DEG C respectively, other operation is the most constant, from
And repetitive operation embodiment 1, thus sequentially it is carried out example 2-3, by the most named for gained composite CL2 and CL3.
Embodiment 4: be not added with investigation during iron compound in step S1
In addition to being omitted by the iron sulfate in step S1, other operation is the most constant, thus repetitive operation embodiment 1,
To embodiment 4, by named for resulting materials CL4.
Embodiment 5-6: the dry investigation with iron compound mass ratio of Fructus Myricae rubrae in step S1
In addition to dry for the Fructus Myricae rubrae in the step S1 mass ratio with iron compound is revised as 5:1 and 20:1 by 10:1, other behaviour
Make the most constant, thus repetitive operation embodiment 1, sequentially obtain embodiment 5-6, by the most named for gained composite CL5 and
CL6。
Embodiment 7-8: the investigation of iron compound in step S1
In addition to the iron sulfate in step S1 is replaced with ferric nitrate and iron chloride respectively, other operation is the most constant, thus weight
Operation embodiment 1, sequentially obtains embodiment 7-8, by the most named for gained composite CL7 and CL8 again.
Microscopic sdIBM-2+2q.p.approach
The material obtaining carbon ball-silicon/iron oxide composite material material CL1 and the embodiment 4 of embodiment 1 gained has carried out many
The microscopic sdIBM-2+2q.p.approach of individual means of different, result is as follows:
1, from Fig. 1-2, described CL1 is the spherical shape of rule, and particle diameter is about 100nm.
2, scheme from the XRS of Fig. 3-4 it can be seen that described CL1 exists containing C element, N element, O element and Fe element,
And ferrum exists in the form of the oxide.
3 and as seen from Figure 11, when reaction system does not adds iron sulfate, then cannot obtain the compound of rule spherical shape
Material, this proof only adds iron compound, just can obtain the spherical composite of rule.
Wherein, in following electrical performance testing, the electrode for capacitors used is all according to above-mentioned " electrode for capacitors
Preparation method " in step (A)-(B) and prepare.
Electrical performance testing
1, Fig. 5 is to use CL1 and prepared electrode for capacitors cyclic voltammogram under different scanning rates.
Wherein, in left hand view, the scanning of top-down three closed circular curves (i.e. peak plays arrangement downwards)
Speed is followed successively by 10mv/s, 5mv/s and 1mv/s；In right part of flg, (i.e. peak rises top-down 4 closed circular curves
Arrangement downwards) sweep speed be followed successively by 1000mv/s, 800mv/s, 400mv/s and 100mv/s.
By this figure it can be seen that this material C L1 still has preferable rectangle, little speed discharge and recharge under the speed of 1000mv/s
There is good rectangle.Under formula calculates at 1000mv/s, capacity can reach 60-70F/g.
2, Fig. 6 is the constant current charge-discharge figure using CL1 and prepared electrode for capacitors under different electric current densities.
Wherein, in left hand view, from the right side, the electric current density on a left side is followed successively by 1A/g, 2A/g, 4A/g, 5A/g and 8A/g；?
In right part of flg, from the right side, the electric current density on a left side is followed successively by 10A/g, 20A/g, 40A/g and 80A/g.
As seen from Figure 6, the discharge and recharge under the multiplying power of 80A/g of this material C L1, electric capacity is computed still having 102.04F/
G, under the multiplying power of 0.5A/g, capacity has 252.09F/g.This prove described material C L1 can in discharge and recharge under high current density,
Show the charge-discharge performance of excellence.
3, Fig. 7 is to use CL1 and the high rate during charging-discharging figure of prepared electrode for capacitors.It may be seen that it is described
Capacitor has the high rate during charging-discharging of excellence, even if under the electric current density of 80A/g, still can have about 120F/G
Electric capacity.
4, Fig. 8 is the Ragone figure using CL1 and prepared electrode for capacitors.From this figure, it can be seen that 0.5A/g's
Under electric current density (uppermost point), the energy density of this material can reach 43.5Wh/L.Under the electric current density of 80A/g,
Power density can reach 45KW/kg.This with it has been reported that material compared with, have higher ability metric density and power close
Degree.
5, Fig. 9 is to use CL1 and prepared electrode for capacitors cyclical stability figure under the electric current density of 80A/g.By
This figure is visible, and this material has extraordinary cyclical stability under high current density, circulation 30000 circle after capacity almost without
Any decay, shows the cyclical stability of excellence.
From above-mentioned Fig. 5-9, the carbon ball-silicon/iron oxide composite material obtained by the inventive method has the electricity of excellence
Performance, thus can be used as the electrode material of capacitor especially ultracapacitor, before electrochemical field has good application
Scape and industrial production potential.
The electric property of other material characterizes
1, Figure 10 is to use the composite of embodiment of the present invention 1-3 respectively and the constant current charge and discharge of prepared electrode for capacitors
Electrograph.Wherein, it is respectively electrode, CL3 (i.e. step S3 prepared by CL1 (i.e. in step S3, treatment temperature is 900 DEG C) from right-to-left
Middle treatment temperature is 1000 DEG C) electrode prepared of the electrode prepared and CL2 (i.e. in step S3, treatment temperature is 800 DEG C).
Through calculating, the place in step S3 corresponding to the capacitance of the electrode prepared by CL1-CL3 and CL1-CL3
Reason temperature is as shown in table 1 below:
Table 1
As can be seen here, in step s3, the temperature of high-temperature process selects extremely important, and wherein 900 DEG C is optimum temperature, this
Time can obtain the composite with optimal performance.
2, Figure 12 be respectively use the embodiment of the present invention 1, the composite of 4-6 and prepared electrode for capacitors exists
Cyclic voltammogram under the sweep speed of 1000mv/s.Wherein, four closed circular curves from bottom to top (minimum light to
Upper arrangement) material that used is respectively CL1 (dry and iron compound the mass ratio of Fructus Myricae rubrae is 10:1), CL6 (Fructus Myricae rubrae is dry with ferrum
The mass ratio of compound is 20:1), CL5 (dry and iron compound the mass ratio of Fructus Myricae rubrae is 5:1) and CL4 (without iron oxides, for
“Blank”)。
Through calculating, the electrode capacitance value such as table 2 below when sweep speed is 1000mv/s, prepared by CL1, CL4-CL6
Shown in, list the dry mass ratio with iron compound of the most corresponding Fructus Myricae rubrae in the lump.
Table 2
As can be seen here, dry when Fructus Myricae rubrae and iron compound mass ratio can obtain having best electric property when being 10:1
Composite, and when deviateing this numerical value, electric property will be caused to be significantly reduced, to be even weaker than and not use any ferrum
(the electrode capacitance value not using the CL4 of any iron compound is 32.2F/g to the performance of material during compound, is higher than on the contrary
CL5)。
3, Figure 13 be respectively use the embodiment of the present invention 1, the composite of 7-8 and prepared electrode for capacitors exists
Cyclic voltammogram under the sweep speed of 1000mv/s.Wherein, three closed circular curves from bottom to top (minimum light to
Upper arrangement) material that used is respectively CL1 (iron sulfate), CL8 (iron chloride) and CL7 (ferric nitrate).
Through calculating, the electrode capacitance value such as table 3 below when sweep speed is 1000mv/s, prepared by CL1, CL7-CL8
Shown in, list the iron compound each used in the lump.
Table 3
As can be seen here, the kind of iron compound has significant impact for the electric property of final composite, wherein, and sulfur
Acid ferrum can obtain effect the most excellent, and other iron compound all causes electric property to be significantly reduced, even if right and wrong
Often similar ferric nitrate or iron chloride, electric property also has and significantly reduces.
As it has been described above, by above-mentioned all embodiments it can be seen that the described preparation method of the present invention is by specific technique
The synergistic combination of step, technological parameter and material selection etc. and coordinative role, thus obtained the carbon with excellent electric property
Ball-silicon/iron oxide composite material, thus may be used on capacitor area, have a good application prospect and industrialization potential.
Should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to limit the protection model of the present invention
Enclose.Additionally, it will also be appreciated that after the technology contents having read the present invention, the present invention can be made respectively by those skilled in the art
Planting change, amendment and/or modification, all these equivalent form of value falls within the guarantor that the application appended claims is limited equally
Within the scope of protecting.
Claims (10)
1. a preparation method for carbon ball-silicon/iron oxide composite material, described method comprises the steps:
S1: Fructus Myricae rubrae is dry, deionized water and iron compound react in high-pressure reactor；
S2: after reaction terminates, pressure release is to normal pressure, and naturally cools to room temperature, washs gained solid, is vacuum dried, done
Dry sample；
S3: described drying sample is carried out under inert gas shielding high-temperature process, thus it is multiple to obtain described carbon ball-iron oxides
Condensation material.
2. preparation method as claimed in claim 1, it is characterised in that: in step sl, described iron compound is ferric nitrate, sulfur
Any one or the most multiple mixture, most preferably iron sulfate in acid ferrum or iron chloride.
3. preparation method as claimed in claim 1 or 2, it is characterised in that: in step sl, the dry matter with iron compound of Fructus Myricae rubrae
Amount ratio is 5-20:1, most preferably 10:1.
4. the preparation method as described in any one of claim 1-3, it is characterised in that: in step sl, Fructus Myricae rubrae does and deionization
The mass ratio of water is 1:1-3.
5. the preparation method as described in any one of claim 1-4, it is characterised in that: in step sl, reaction temperature is 160-
220℃。
6. the preparation method as described in any one of claim 1-5, it is characterised in that: in step s3, described high-temperature process
Temperature is 800-1000 DEG C, most preferably 900 DEG C.
7. the carbon ball-silicon/iron oxide composite material obtained by preparation method described in any one of claim 1-6.
8. carbon ball described in claim 7-silicon/iron oxide composite material purposes in preparing capacitor.
9. a preparation method for electrode for capacitors, described method comprises the steps:
(A) weigh the composite described in claim 7, acetylene black, (three's mass ratio is PTFE (politef) emulsion
80:10:10), add ethanol in proper amount, mix homogeneously, when being stirred continuously into starchiness, be coated onto in nickel foam；
(B) nickel foam coating described composite is dried, dries, tabletting, i.e. obtain described electrode for capacitors.
10. one kind comprises the electrode for capacitors of carbon ball-silicon/iron oxide composite material described in claim 7.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112830488A (en) * | 2021-02-03 | 2021-05-25 | 安徽工程大学 | Catalyst-free preparation method and application of porous spiral carbon material |
| CN113903602A (en) * | 2021-09-24 | 2022-01-07 | 华南师范大学 | Preparation method and application of osmanthus leaf composite electrode |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1567493A (en) * | 2003-07-03 | 2005-01-19 | 中国科学院电工研究所 | A composite carbon-based electrode material for super capacitor and method for making same |
| CN1971786A (en) * | 2005-11-25 | 2007-05-30 | 中国科学院金属研究所 | An electrochemical capacitor electrode material and its preparing method |
| CN104766963A (en) * | 2015-04-22 | 2015-07-08 | 安徽理工大学 | Method for preparing metal oxide-carbon fiber nano composite material |
-
2016
- 2016-05-11 CN CN201610312374.6A patent/CN106057486B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1567493A (en) * | 2003-07-03 | 2005-01-19 | 中国科学院电工研究所 | A composite carbon-based electrode material for super capacitor and method for making same |
| CN1971786A (en) * | 2005-11-25 | 2007-05-30 | 中国科学院金属研究所 | An electrochemical capacitor electrode material and its preparing method |
| CN104766963A (en) * | 2015-04-22 | 2015-07-08 | 安徽理工大学 | Method for preparing metal oxide-carbon fiber nano composite material |
Non-Patent Citations (6)
| Title |
|---|
| JUN PU 等: "Fe3O4@C core–shell microspheres synthesis, characterization, and application as supercapacitor electrodes", 《JOURNAL OF SOLID STATE ELECTROCHEMISTRY》 * |
| KANG UK LEE 等: "Catalytic growth of a colloidal carbon sphere by hydrothermal reaction with iron oxide (Fe3O4) catalyst", 《MATERIALS LETTERS》 * |
| SHIBING NI 等: "Designed synthesis of wide range microwave absorption Fe3O4–carbon sphere composite", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| YUXIAN WANG 等: "Magnetic Fe3O4/carbon spherecobalt composites for catalytic oxidation of phenol solutions with sulfate radicals", 《CHEMICAL ENGINEERING JOURNAL》 * |
| 刘娇: "纳米四氧化三铁的合成及其电容性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 王梦姣: "以生物质为源的多孔碳及其复合物的制备以及其电化学性能的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112830488A (en) * | 2021-02-03 | 2021-05-25 | 安徽工程大学 | Catalyst-free preparation method and application of porous spiral carbon material |
| CN113903602A (en) * | 2021-09-24 | 2022-01-07 | 华南师范大学 | Preparation method and application of osmanthus leaf composite electrode |
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