CN105609320B - The preparation method of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material - Google Patents
The preparation method of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material Download PDFInfo
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Abstract
A kind of preparation method of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material is from biomass catkin that is clean, drying; it is placed in tubular type retort; inert gas is passed through as protection gas, then high-temperature heat treatment, is made Carbon Hollow micron tube；From nickel acetate, cobalt acetate and thiocarbamide are dissolved in organic solvent, and mixed solution is made, and Carbon Hollow micron tube is then added into mixed solution, is sufficiently stirred, and are well mixed；Hydro-thermal reaction is carried out, reaction naturally cools to room temperature after terminating, and centrifuges, and filters, and washs, and dries, and Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material is made.The present invention has the advantages of specific capacity is high, and multiplying power property is excellent.
Description
Technical field
The invention belongs to a kind of preparation method of capacitor electrode material, and in particular to a kind of biomass-based Carbon Hollow micron
The preparation method of pipe/nickel cobalt metal sulfide combination electrode material
Background technology
Biomass catkin is a kind of common environmental contaminants, is especially caused seriously to natural environment in season the end of spring and the beginning of summer
Pollution, and brings inconvenience to the trip of people, can also make one to cause such as breathing problem and it is allergic the problems such as.
However, catkin, as a kind of natural, being recycled acquisition, cheap biomass castoff, its microstructure is that one kind has
The biomass fiber of high degree of hollowness.Using the distinctive microcosmos structure characteristic of the biomass, it is carried out under inert atmosphere conditions
High-temperature heat treatment, Carbon Hollow micron tube of the degree of hollowness more than 80% can be prepared, be to realize that waste effectively utilizes, be inexpensive
Prepare the effective ways of Carbon Hollow micron tube.
Metal sulfide such as cobalt sulfide, nickel sulfide etc., due to high theoretical specific capacity, abundant redox reaction
Active site, low cost and hypotoxicity, it is all to be widely used in fuel cell, solar cell, lithium ion battery, ultracapacitor etc.
It is multi-field.Compared to binary metal sulfide cobalt sulfide, nickel sulfide, ternary nickel cobalt metal sulfide have higher specific capacity and
More preferable cycle life, huge potentiality are shown in terms of high-performance super capacitor application of electrode.But with Carbon Materials phase
Than metal sulfide is due to its low electric conductivity and multiplying power property is relatively poor.
Therefore, the Carbon Hollow micron tube and ternary nickel cobalt gold with excellent conductive capability that will be prepared by high-temperature heat treatment
It is compound to belong to sulfide progress, is prepared for high performance Carbon Hollow micron tube/nickel cobalt metal sulfide composite, the composite
Have both the high conductivity of Carbon Hollow micron tube and the height ratio capacity characteristic of nickel cobalt metal sulfide, be applied to ultracapacitor
Electrode, excellent chemical property is shown, be a kind of reliable Novel super capacitor electrode material.Found no through retrieval
Same or analogous prior art.
The content of the invention
High, the excellent biomass-based Carbon Hollow micron tube/nickel of multiplying power property it is an object of the invention to provide a kind of specific capacity
The preparation method of cobalt metal sulfide combination electrode material.
The present invention is using biomass castoff catkin as charcoal material precursor, under the conditions of inert atmosphere and certain temperature at heat
Reason, Carbon Hollow micron tube is made.With nickel acetate Ni (CH3COO)2·4H2O is nickel source, cobalt acetate Co (CH3COO)2·4H2O is cobalt
Source, thiocarbamide are sulphur source, are dissolved in organic solvent, are configured to mixed solution, then added into mixed solution it is a certain amount of in
Empty charcoal micron tube, it is sufficiently stirred after making it well mixed, is transferred to closed in water heating kettle, one section of constant temperature under the conditions of certain temperature
Time, room temperature is naturally cooled to, obtain solidliquid mixture, centrifuged, filtered, washed, dried, Carbon Hollow micron tube/nickel cobalt is made
Metal sulfide combination electrode material.The combination electrode material has both the high conductivity of Carbon Hollow micron tube and nickel cobalt metal vulcanizes
The height ratio capacity characteristic of thing, it is a kind of reliable Novel super capacitor electrode material.
The preparation method of the present invention comprises the following steps：
(1) from biomass catkin that is clean, drying, it is placed in tubular type retort, is passed through inert gas and is used as protection gas,
Then high-temperature heat treatment, Carbon Hollow micron tube is made；
(2) nickel, cobalt precursor mixed solution are prepared, from nickel acetate Ni (CH3COO)2·4H2O, cobalt acetate Co
(CH3COO)2·4H2O and thiocarbamide are dissolved in organic solvent, and mixed solution is made, and it is micro- that Carbon Hollow is then added into mixed solution
Mitron, it is sufficiently stirred, is well mixed；
(3) mixture of step (2) being subjected to hydro-thermal reaction, reaction naturally cools to room temperature after terminating, and centrifuges, filtering,
Washing, dry, Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material is made.
Inert atmosphere in the step (1) is N2Or one kind in Ar.
The flow velocity of gas is 2-10ml min in the step (1)-1g-1。
Heat treatment temperature in the step (1) is 700-1000 DEG C, and the rate of heat addition is 5-10 DEG C of min-1, constant temperature time
For 1-3h.
The organic solvent selected in the step (2) is absolute ethyl alcohol, one or both of ethylene glycol in any proportion
The mixed solution of mixing.
Ni in the step (2)2+、Co2+Total ion concentration is 0.01-0.03mol L-1, Ni2+With Co2+Ion concentration
For 1:4~4:Between 1, thiourea concentration Ni2+、Co2+2-4 times of total ion concentration.
Carbon Hollow micron tube quality is 1/2 to 2 times of nickel acetate and cobalt acetate quality summation in the step (2).
Hydro-thermal reaction in the step (3) is carried out in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, water heating kettle highest heatproof 300
DEG C, sample filling degree is the 60-80vol% of polytetrafluoroethylene (PTFE) hydrothermal reaction kettle volume.Reaction temperature is 150-200 DEG C, reaction
Time is 5-15h.
The speed of step (3) centrifugation is 7000-9000rpm, centrifugation time 10-30min.
Washing uses deionized water and ethanol solution in the step (3), is fully washed with ethanol solution first
Wash 2-3 times, be then washed with deionized again 3-4 times.
Drying is that 3-5h is dried at 80-100 DEG C in the step (3).
Carbon Hollow micron tube prepared by the present invention/nickel cobalt metal sulfide combination electrode material institute nickel and cobalt containing metal sulfide
Mass fraction be 30-70wt.%.
Advantages of the present invention is as follows：
(1) present invention uses biomass castoff catkin cheap and easy to get to prepare Carbon Hollow micron tube, cost for presoma
It is low, it is green, make its Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode prepared that there is very high price advantage simultaneously
And show excellent chemical property；
(2) by controlling and adjusting different precursor amounts, concentration, to prepare different crystal forms Jie Gou ﹑ difference depositions
Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material；
(3) preparation method of the present invention is simple, science, can the high performance electrode material for super capacitor of prepare with scale, no
The efficient utilization of environmental waste catkin is only realized, it is big in ultracapacitor industry to also solve nickel cobalt metal sulfide
The problem of sizable application difficulty；
(4) Carbon Hollow micron tube/Ni prepared by the present invention2CoS4Combination electrode material is in 0.5A g-1Under current density, than
Capacity can reach 1230F g-1,10A g-1Specific capacity is 1014F g under current density-1, capacity retention 85.6%.And
Pure Ni2CoS4Electrode material is in 0.5A g-1Under current density, specific capacity is 1046F g-1, 10A g-1Specific capacity under current density
For 786F g-1, capacity retention is only 75.1%.Show that the chemical property of combination electrode material vulcanizes better than pure nickel cobalt metal
The chemical property of thing electrode material.
Brief description of the drawings
Fig. 1 is Carbon Hollow micron tube (Fig. 1 a) and Carbon Hollow micron tube/Ni prepared by embodiment 12CoS4Combination electrode material
The SEM photograph of (Fig. 1 b)；
Fig. 2 is Carbon Hollow micron tube/Ni prepared by embodiment 12CoS4The TEM photos of combination electrode material；
Fig. 3 is Carbon Hollow micron tube/Ni prepared by embodiment 12CoS4The adsorption desorption curve map of combination electrode material；
Fig. 4 is Carbon Hollow micron tube/Ni prepared by embodiment 12CoS4The pore size distribution curve figure of combination electrode material；
Fig. 5 is Carbon Hollow micron tube/Ni prepared by embodiment 12CoS4Combination electrode material specific capacity is with current density change
Picture.
Embodiment
Embodiment 1
(1) 5g biomass catkins are placed in tubular type retort, are passed through Ar and are controlled as protection gas, gas flow rate in 5ml
min-1g-1, with 5 DEG C of min-1The rate of heat addition is warming up to 1000 DEG C, constant temperature 2h, naturally cools to room temperature, obtains Carbon Hollow micron
Pipe.
(2) raw acetic acid nickel (CH is weighed3COO)2·4H2O (1.2mmol), cobalt acetate Co (CH3COO)2·4H2O
(0.6mmol), thiocarbamide (3.6mmol) are dissolved in 60ml absolute ethyl alcohols, and mixed solution is made, is then added into mixed solution
Mesoporous carbon micron tube made from 150mg above-mentioned steps (1), magnetic agitation 2h, it is well mixed.
(3) said mixture is transferred in the polytetrafluoroethylene (PTFE) water heating kettle that volume is 100ml, hydrothermal reaction kettle is placed in drum
In wind baking oven, constant temperature 8h, is subsequently cooled to room temperature at 180 DEG C, centrifuges 10min with 9000rpm rotating speed, then uses absolute ethyl alcohol
Solution fully washs 3 times, then is washed with deionized 3 times, 80 DEG C of dry 5h, and Carbon Hollow micron tube/metal sulfide is made
(Ni2CoS4) combination electrode material.The mass fraction of the combination electrode material institute nickel and cobalt containing metal sulfide is 70wt.%,
0.5A g-1Under current density, specific capacity can reach 1230F g-1,10A g-1Specific capacity is 1014F g under current density-1, electricity
It is 85.6% to hold conservation rate, shows superior high rate performance.
Embodiment 2
(1) 5g biomass catkins are placed in tubular type retort, are passed through Ar and are controlled as protection gas, gas flow rate in 7ml
min-1g-1, with 7 DEG C of min-1The rate of heat addition is warming up to 700 DEG C, constant temperature 1.5h, naturally cools to room temperature, obtains Carbon Hollow micron
Pipe.
(2) raw acetic acid nickel (CH is weighed3COO)2·4H2O (0.9mmol), cobalt acetate Co (CH3COO)2·4H2O
(0.9mmol), thiocarbamide (4.5mmol) are dissolved in 80ml absolute ethyl alcohols, and mixed solution is made, is then added into mixed solution
Mesoporous carbon micron tube made from 200mg above-mentioned steps (1), magnetic agitation 3h, it is well mixed.
(3) said mixture is transferred in 100ml polytetrafluoroethylene (PTFE) water heating kettles, hydrothermal reaction kettle is placed in convection oven
In, constant temperature 10h, is subsequently cooled to room temperature at 170 DEG C, centrifuges 20min with 8000rpm rotating speed, then uses ethanol solution
Fully washing 2 times, then be washed with deionized 3 times, 90 DEG C of dry 4h, Carbon Hollow micron tube/nickel cobalt metal sulfide is made and answers
Composite electrode material.The mass fraction of the combination electrode material institute nickel and cobalt containing metal sulfide is 60wt.%, in 0.5A g-1Electric current
Under density, specific capacity can reach 1140F g-1, 10A g-1Specific capacity is 952F g under current density-1, capacity retention is
83.5%.
Embodiment 3
(1) 8g biomass catkins are placed in tubular type retort, are passed through N2As protection gas, gas flow rate is controlled in 8ml
min-1g-1, with 10 DEG C of min-1The rate of heat addition is warming up to 1000 DEG C, constant temperature 3h, naturally cools to room temperature, obtains Carbon Hollow micron
Pipe.
(2) raw acetic acid nickel (CH is weighed3COO)2·4H2O (0.6mmol), cobalt acetate Co (CH3COO)2·4H2O
(1.2mmol), thiocarbamide (5.4mmol) are dissolved in 80ml ethylene glycol, and mixed solution is made, is then added into mixed solution
Mesoporous carbon micron tube made from 300mg above-mentioned steps (1), magnetic agitation 3h, it is well mixed.
(3) said mixture is transferred in 100ml polytetrafluoroethylene (PTFE) water heating kettles, hydrothermal reaction kettle is placed in convection oven
In, 200 DEG C of constant temperature 5h, room temperature is subsequently cooled to, 30min is centrifuged with 7000rpm rotating speed, it is then abundant with ethanol solution
Washing 3 times, then be washed with deionized 3 times, 100 DEG C of dry 3h, Carbon Hollow micron tube/nickel cobalt metal sulfide compound electric is made
Pole material.The mass fraction of the combination electrode material institute nickel and cobalt containing metal sulfide is 40wt.%, in 0.5A g-1Current density
Under, its specific capacity can reach 938F g-1,10A g-1Specific capacity is 746F g under current density-1, capacity retention is
79.5%.
Embodiment 4
(1) 6g biomass catkins are placed in tubular type retort, are passed through N2As protection gas, gas flow rate is controlled in 10ml
min-1g-1, with 6 DEG C of min-1The rate of heat addition is warming up to 800 DEG C, constant temperature 3h, naturally cools to room temperature, obtains Carbon Hollow micron tube.
(2) raw acetic acid nickel (CH is weighed3COO)2·4H2O (1.44mmol), cobalt acetate Co (CH3COO)2·4H2O
(0.36mmol), thiocarbamide (6.9mmol) are dissolved in 70ml ethylene glycol, and mixed solution is made, is then added into mixed solution
Mesoporous carbon micron tube made from 250mg above-mentioned steps (1), magnetic agitation 2h, it is well mixed.
(3) said mixture is transferred in 100ml polytetrafluoroethylene (PTFE) water heating kettles, hydrothermal reaction kettle is placed in convection oven
In, 160 DEG C of constant temperature 12h, room temperature is subsequently cooled to, 30min is centrifuged with 7500rpm rotating speed, then filled with ethanol solution
Divide washing 2 times, then be washed with deionized 4 times, 80 DEG C of dry 5h, it is compound that Carbon Hollow micron tube/nickel cobalt metal sulfide is made
Electrode material.The mass fraction of the combination electrode material institute nickel and cobalt containing metal sulfide is 50wt.%, in 0.5A g-1Electric current is close
Under degree, specific capacity can reach 1310F g-1,10A g-1Specific capacity is 1043F g under current density-1, capacity retention is
79.6%.
Embodiment 5
(1) 10g biomass catkins are placed in tubular type retort, are passed through N2As protection gas, gas flow rate is controlled in 2ml
min-1g-1, with 6 DEG C of min-1The rate of heat addition is warming up to 900 DEG C, constant temperature 1h, naturally cools to room temperature, obtains Carbon Hollow micron tube.
(2) raw acetic acid nickel (CH is weighed3COO)2·4H2O (0.64mmol), cobalt acetate Co (CH3COO)2·4H2O
(0.16mmol), thiocarbamide (3.2mmol) are dissolved in 80ml ethylene glycol, and mixed solution is made, is then added into mixed solution
Mesoporous carbon micron tube made from 200mg above-mentioned steps (1), magnetic agitation 2h, it is well mixed.
(3) said mixture is transferred in 100ml polytetrafluoroethylene (PTFE) water heating kettles, hydrothermal reaction kettle is placed in convection oven
In, 150 DEG C of constant temperature 15h, room temperature is subsequently cooled to, 20min is centrifuged with 8000rpm rotating speed, then filled with ethanol solution
Divide washing 3 times, then be washed with deionized 4 times, 90 DEG C of dry 4h, it is compound that Carbon Hollow micron tube/nickel cobalt metal sulfide is made
Electrode material.The mass fraction of the combination electrode material institute nickel and cobalt containing metal sulfide is 30wt.%, in 0.5A g-1Electric current is close
Under degree, specific capacity is 780F g-1, 10A g-1Specific capacity is 642F g under current density-1, capacity retention 82.3%.
Claims (10)
1. a kind of preparation method of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material, its feature exist
In comprising the following steps：
（1）From biomass catkin that is clean, drying, it is placed in tubular type retort, is passed through inert gas as gas is protected, then
High-temperature heat treatment, Carbon Hollow micron tube is made；
（2）Nickel, cobalt precursor mixed solution are prepared, from nickel acetate, cobalt acetate and thiocarbamide are dissolved in organic solvent, and mixing is made
Solution, Carbon Hollow micron tube is then added into mixed solution, is sufficiently stirred, be well mixed；
（3）By step（2）Mixture carry out hydro-thermal reaction, reaction terminate after naturally cool to room temperature, centrifuge, filter, washing,
Dry, Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material is made；
The step（2）Middle Ni2+、Co2+Total ion concentration is 0.01-0.03 mol L-1, Ni2+With Co2+Ion concentration is 1:4
~4:Between 1, thiourea concentration Ni2+、Co2+2-4 times of total ion concentration；
The step（2）Middle Carbon Hollow micron tube quality is 1/2 to 2 times of nickel acetate and cobalt acetate quality summation.
2. a kind of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material as claimed in claim 1
Preparation method, it is characterised in that the step（1）The flow velocity of middle gas is 2-10 ml min-1 g-1。
3. a kind of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material as claimed in claim 1
Preparation method, it is characterised in that the step（1）In heat treatment temperature be 700-1000oC, rate of heat addition 5-10oC
min-1, constant temperature time is 1-3 h.
4. a kind of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material as claimed in claim 1
Preparation method, it is characterised in that the step（1）In inert atmosphere be N2Or one kind in Ar.
5. a kind of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material as claimed in claim 1
Preparation method, it is characterised in that the step（2）The organic solvent of middle selection is absolute ethyl alcohol, one kind in ethylene glycol or two
Kind.
6. a kind of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material as claimed in claim 1
Preparation method, it is characterised in that the step（3）In hydro-thermal reaction carried out in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, sample dress
Degree of filling out is the 60-80vol%, reaction temperature 150-200 of polytetrafluoroethylene (PTFE) hydrothermal reaction kettle volumeoC, reaction time 5-15
h。
7. a kind of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material as claimed in claim 1
Preparation method, it is characterised in that the step（3）The speed of centrifugation is 7000-9000 rpm, centrifugation time 10-30min.
8. a kind of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material as claimed in claim 1
Preparation method, it is characterised in that the step（3）Middle washing uses deionized water and ethanol solution, uses absolute ethyl alcohol first
Solution fully washs 2-3 times, is then washed with deionized again 3-4 times.
9. a kind of biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide combination electrode material as claimed in claim 1
Preparation method, it is characterised in that the step（3）Middle drying is in 80-100o3-5 h are dried under C.
A kind of 10. biomass-based Carbon Hollow micron tube/nickel cobalt metal sulfide compound electric as described in claim any one of 1-9
The preparation method of pole material, it is characterised in that contained by the Carbon Hollow micron tube of preparation/nickel cobalt metal sulfide combination electrode material
The mass fraction of nickel cobalt metal sulfide is 30-70wt%.
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| CN106568815B (en) * | 2016-10-21 | 2018-10-16 | 西安建筑科技大学 | A kind of cobalt nickel bimetal sulfide organophosphorus pesticide biosensor and preparation method |
| CN106992078A (en) * | 2017-03-02 | 2017-07-28 | 同济大学 | The preparation method of porous carbon/transiton metal binary oxides micro-sphere material |
| CN108695076B (en) * | 2018-05-21 | 2019-08-23 | 青岛大学 | A kind of preparation method and applications of the capacitor material of 3D hollow structure |
| CN110060873B (en) * | 2019-04-17 | 2020-12-08 | 齐鲁工业大学 | Hollow biochar sphere-based nickel sulfide nanorod supercapacitor and preparation method thereof |
| CN110028066B (en) * | 2019-05-09 | 2021-03-26 | 中国科学院山西煤炭化学研究所 | Preparation method of porous carbon micro-tube and porous carbon micro-tube |
| CN110002429B (en) * | 2019-05-09 | 2020-12-01 | 中国科学院山西煤炭化学研究所 | Carbon nanotube/transition metal hydroxide composite electrode material and preparation method thereof |
| CN110660968A (en) * | 2019-09-17 | 2020-01-07 | 天津大学 | Composite lithium metal negative electrode and preparation method thereof |
| CN113026050B (en) * | 2021-03-04 | 2022-04-05 | 哈尔滨工程大学 | Carbonized common sow thistle loaded Ni-doped MoS2 electrode material |
| CN114583127B (en) * | 2022-02-28 | 2023-05-09 | 南京工业大学 | Method for preparing CoNi-S@3D-C nanocomposite and modified battery diaphragm |
| CN115894876B (en) * | 2022-12-30 | 2024-03-19 | 河南金丹乳酸科技股份有限公司 | AA and BDO esterification process for PBAT production |
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| CN102086034B (en) * | 2010-12-13 | 2012-10-24 | 南京邮电大学 | Carbon-nano-tube prepared from poplar catkin and willow catkin as raw materials and preparation method |
| CN104616900B (en) * | 2015-01-23 | 2017-11-10 | 三峡大学 | A kind of cobalt nickel bimetal sulfide, preparation method and applications |
| CN104795245A (en) * | 2015-05-14 | 2015-07-22 | 安徽师范大学 | Wire-shaped nickel cobalt oxide@nickel cobalt sulfide hetero-structure composite, and preparation method and purpose thereof |
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