CN107610939A - A kind of nano-cellulose base flexible composite electrode material and preparation method thereof - Google Patents
A kind of nano-cellulose base flexible composite electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to electrode material preparing technical field, discloses a kind of nano-cellulose base flexible composite electrode material and preparation method thereof.The preparation method is：By nano-cellulose, graphene, active material is added or be added without, is added to after mixing in distilled water and is well mixed, is beaten, being ultrasonically treated, obtain mixed slurry；Then gained mixed slurry is manufactured paper with pulp shaping by wet papermaking process, the nano-cellulose base flexible composite electrode material is obtained after drying.Invention prepares flexible composite electrode material using the technique shaping of manufacturing paper with pulp of wet papermaking, the flexibility, intensity and excellent chemical property of electrode material can be ensured, on the basis of possessing certain flexibility, bending fold several times after, electrode material internal structure and its specific capacity can well be kept；After recycling several times, its specific capacity remains to keep good.
Description
Technical field
The invention belongs to electrode material preparing technical field, and in particular to a kind of nano-cellulose base flexible compound electrode material
Material and preparation method thereof.
Background technology
With the development of science and technology, flexible electronic product fast development, lightweight, flexibility, foldable electronic device one
When become the object of researcher's research, and to develop corresponding flexible energy storage equipment accordingly.2009, can
Flexible basic technology enters research and development into the research of scalable energy storage device from medical science value, and 2013, U.S. northwest was big
Huang Yonggang professors and the John A.Rogers professors of the University of Illinois in the U.S. deliver on Nat.Commun. magazines
The article of one electrode structure on flexible expandable battery.At present, researchers are to flexible electronic devices and flexibility
Energy storage equipment research is more and more deep.
Wet papermaking process technology is very ripe in China, and at present, cylinder mould machine and oblique net paper machine are production speciality paper
Indispensable process equipment, the advantages of respective is suffered from, the pulling force in length and breadth of cylinder mould machine page is smaller, is adapted to small yield
The production of speciality paper, cylinder mould machine online concentration is low, and the formation of sheet of production is good, and air permeability is high, but uses wet papermaking at present
Technique prepare flexible electrode material be but rarely reported.
Cellulose be on the earth enrich renewable resource, it is degradable, green, possess good filming performance and
Pliability, nano-cellulose is not only green renewable as general fibre element, and possesses more excellent because size is small
The performances such as different mechanics, optics, calorifics so that nano-cellulose all finds application in numerous areas.
Ultracapacitor combines the advantage of battery and traditional capacitor, the high energy density and power density having,
Further, since its advantages that discharge and recharge time is short, cyclical stability is high by the stand-by power supply as many instrument and equipments, it is extensive
It is used in the various fields such as energy device, power.And lithium ion battery possesses the advantages that high-energy-density, high power capacity.Prepare
Development of the flexible ultracapacitor and lithium ion battery electrode material to electrode material is significant.
The content of the invention
In place of shortcoming and defect existing for above prior art, primary and foremost purpose of the invention is to provide a kind of nanometer
The preparation method of cellulose base flexible composite electrode material.
It is flexible multiple another object of the present invention is to provide a kind of nano-cellulose base being prepared by the above method
Composite electrode material.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of nano-cellulose base flexible composite electrode material, including following preparation process：
(1) by nano-cellulose, graphene, active material is added or be added without, is added in distilled water and mixes after mixing
Close uniform, mashing, be ultrasonically treated, obtain mixed slurry；
(2) mixed slurry obtained by step (1) is manufactured paper with pulp shaping by wet papermaking process, the Nanowire is obtained after drying
Tie up plain base flexible composite electrode material.
Preferably, described nano-cellulose size is 10~100nm, and described graphene refers to single-layer graphene.
Preferably, described active material is at least one in manganese dioxide, polyaniline, aluminium titanates and ferrous phosphate aluminium
Kind.
Preferably, described shaping of manufacturing paper with pulp refers to shaping of being manufactured paper with pulp on cylinder mould machine or oblique net paper machine, and shaping of manufacturing paper with pulp is determined
Measure as 5~30g/m2, thickness is 10~100 μm.
Preferably, the temperature of the drying is 105 DEG C.
A kind of nano-cellulose base flexible composite electrode material, is prepared by the above method.
Nano-cellulose crystallinity that the present invention uses is high, excellent in mechanical performance, and support is played in whole electrode material
The effect of enhancing.
Graphene is to be stacked to form by carbon atom, with sp2The mode of hydridization arranges, and is a kind of individual layer, cellular crystalline substance
Body, because its special structure causes it to possess the performances such as excellent mechanics, electricity, its specific surface area is big, there is excellent pair
Electric layer capacitive property.
Manganese dioxide of super capacitor electrode material and polyaniline cost are low, there is excellent fake capacitance performance, this hair
It is bright to be mixed with flexible composite electrode material using manganese dioxide, polyaniline and graphene, it is excellent that performance graphene can be integrated
Electric double layer capacitance performance and the excellent fake capacitance performance of manganese dioxide, polyaniline so that the overall electrification of combination electrode material
Performance is learned to be greatly enhanced.Li-ion electrode materials lithium titanate and LiFePO 4 have high-energy, high power capacity etc. excellent
Point, play both common advantages with reference to graphene and the specific capacity of lithium ion battery electrode material totality is improved.
The present invention preparation method and resulting product has the following advantages that and beneficial effect：
(1) present invention manufactures paper with pulp to be molded using the technique of wet papermaking on cylinder mould machine or oblique net paper machine prepares flexible compound
Electrode material, the flexibility, intensity and excellent chemical property of electrode material can be ensured, it will be made to be prepared on a large scale
Production, the research to flexible electrode material are significant with preparation；
(2) the property combination electrode material prepared by the present invention is on the basis of possessing certain flexibility, and bending fold is several times
Afterwards, electrode material internal structure and its specific capacity can well be kept；After recycling several times, its specific capacity
Remain to keep good.
Brief description of the drawings
Fig. 1 is that (A is pulp distributor in figure, and B is rectification for the structural representation of the oblique net paper machine used in the embodiment of the present invention
Area, C are drainage and formation area, and D is the flexible composite electrode material after shaping).
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) by 30wt% nano-celluloses and 70wt% single-layer graphenes (model SE1233, powdered, manufacturer
For the hexa-atomic element in Changzhou) mixing after add distilled water, be added in mixer and be beaten, the mixed liquor being beaten is added to cell
It is ultrasonically treated 15 minutes in disintegrating machine, further processing make it that the particle diameter of nano-cellulose and graphene is smaller, disperses more
Uniformly.
(2) mixed slurry after supersound process is added to wet method on oblique net paper machine as shown in Figure 1 and manufactures paper with pulp shaping (in figure
A is the pulp distributor of oblique net paper machine, and slurry, which enters, will not wherein mix；B be oblique net paper machine commutating zone, the effect of commutating zone
It is the flow regime for the slurry rectification for coming from pulp distributor being produced high-strength micro-turbulence, does not produce vortex, so that the fluidised form of slurry
It is stable, to ensure that slurry does not mix when shaping and obtains the good uniformity；Slurry after commutating zone by arriving
Up at the drainage and formation area C of oblique net paper machine, by being freely dehydrated or certain vacuum dehydration makes the slurry that comes from commutating zone
The successively dehydration forming at drainage and formation area C；D is the flexible composite electrode material after shaping), applying pressure during shaping is
0.5Mpa, quantification of 30g/m2, thickness is 60 μm~100 μm, then puts the flexible composite electrode material film layer peeled
Enter in blast drier and be dried, drying temperature is 105 DEG C, obtains the nano-cellulose base flexible composite electrode material.
Embodiment 2
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 40wt% nano-celluloses and 60wt% single-layer graphenes with part, other steps are identical.
Embodiment 3
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 50wt% nano-celluloses and 50wt% single-layer graphenes with part, other steps are identical.
Embodiment 4
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 60wt% nano-celluloses and 40wt% single-layer graphenes with part, other steps are identical.
Embodiment 5
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 70wt% nano-celluloses and 30wt% single-layer graphenes with part, other steps are identical.
The performance test results such as institute of table 1 of the gained nano-cellulose base flexible composite electrode material of above example 1~5
Show：
Table 1
| Embodiment | Modulus of elasticity (Mpa) | Specific capacity (F/g) | Surface resistance (Ω/sq) |
| 1 | 3184.48 | 116.84 | 9.51 |
| 2 | 3315.34 | 87.23 | 11.62 |
| 3 | 4184.26 | 76.14 | 17.57 |
| 4 | 3639.52 | 52.46 | 25.03 |
| 5 | 3375.87 | 41.37 | 41.50 |
After the folding of the gained nano-cellulose base flexible composite electrode material of above example 1~5 and cycle charge-discharge 1000
The performance test results it is as shown in table 2：
Table 2
Specific capacitance value of the gained nano-cellulose base flexible composite electrode material of above example 1 under different scanning rates
Test result is as shown in table 3：
Table 3
| Sweep speed (mv/s) | 10 | 30 | 50 | 70 | 90 |
| Specific capacitance value (F/g) | 116.84 | 84.53 | 57.39 | 31.86 | 15.43 |
It is to be measured in sweep speed under conditions of 10mv/s with the property indices in upper table 1, table 2.
The Elastic Modulus of embodiment 1 has also reached a higher value as can be seen from Table 1, composite specific capacitance and
Surface resistance is superior to other embodiment, i.e. graphene dosage is more than nano-cellulose dosage, and it can be made to possess a larger ratio
Capacity and relatively low surface resistance, it is a preferred embodiment.
Fold 1000 times as can be seen from Table 2 and cycle charge-discharge 1000 times after, prepared by embodiment 1~5 receives
The property indices of rice cellulose base flexible composite electrode material keep preferable.
As can be seen from Table 3, the present invention gained nano-cellulose base flexible composite electrode material specific capacitance value by
Sweep speed has a great influence, and flexible composite electrode material performance under low sweep speed can show more preferable, the electrode material life-span
Can be longer.
Embodiment 6~11 is the preparation embodiment of ultracapacitor nano-cellulose base flexible composite electrode material：
Embodiment 6
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 50wt% single-layer graphenes and 20wt% manganese dioxide with part, other steps are complete
It is exactly the same.
Embodiment 7
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 40wt% single-layer graphenes and 30wt% manganese dioxide with part, other steps are complete
It is exactly the same.
Embodiment 8
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 30wt% single-layer graphenes and 40wt% manganese dioxide with part, other steps are complete
It is exactly the same.
The performance test results such as institute of table 4 of the gained nano-cellulose base flexible composite electrode material of above example 6~8
Show：
Table 4
| Embodiment | Modulus of elasticity (Mpa) | Specific capacity (F/g) | Surface resistance (Ω/sq) |
| 6 | 3064.27 | 174.67 | 12.60 |
| 7 | 2985.87 | 128.83 | 21.14 |
| 8 | 2874.39 | 114.36 | 34.20 |
The gained nano-cellulose base flexible composite electrode material of above example 6~8 folds and cycle charge-discharge 1000 times
The performance test results afterwards are as shown in table 5：
Table 5
It is to be measured in sweep speed under conditions of 10mv/s with the property indices in upper table 4, table 5.
As can be seen from Table 4, on the basis of embodiment 1~5, embodiment 6~8 is a part of manganese dioxide of addition
Afterwards, the nano-cellulose base flexible composite electrode material that wet moulding obtains, specific capacity improve much than embodiment 1~5, this
It is the result of manganese dioxide fake capacitance and graphene electric double layer capacitance comprehensive function, adding a small amount of manganese dioxide can effectively improve again
The combination property of composite electrode material.
As can be seen from Table 5, the nano-cellulose base flexible composite electrode material that prepared by embodiment 6~8 passes through
After 1000 foldings and 1000 cycle charge-discharges, various aspects of performance index can keep preferable.
Embodiment 9
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 50wt% single-layer graphenes and 20wt% polyanilines with part, other steps are complete
It is identical.
Embodiment 10
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 40wt% single-layer graphenes and 30wt% polyanilines with part, other steps are complete
It is identical.
Embodiment 11
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 30wt% single-layer graphenes and 40wt% polyanilines with part, other steps are complete
It is identical.
The performance test results such as institute of table 6 of the gained nano-cellulose base flexible composite electrode material of above example 9~11
Show：
Table 6
| Embodiment | Modulus of elasticity (Mpa) | Specific capacity (F/g) | Surface resistance (Ω/sq) |
| 9 | 3464.27 | 92.30 | 16.73 |
| 10 | 3985.87 | 107.80 | 18.49 |
| 11 | 3874.39 | 150.36 | 24.45 |
The gained nano-cellulose base flexible composite electrode material of above example 9~11 folds and cycle charge-discharge 1000 times
The performance test results afterwards are as shown in table 7：
Table 7
It is to be measured in sweep speed under conditions of 10mv/s with the property indices in upper table 6, table 7.
As can be seen from Table 6, on the basis of embodiment 1~5, embodiment 9~11 add polyaniline after, wet method into
The nano-cellulose base flexible composite electrode material that type obtains, specific capacity improve much than embodiment 1~5, and this is polyaniline
Fake capacitance and the result of graphene electric double layer capacitance comprehensive function, combination electrode material can be effectively improved by adding part polyaniline
Combination property.
As can be seen from Table 7, the nano-cellulose base flexible composite electrode material that prepared by embodiment 9~11 passes through
After 1000 foldings and 1000 cycle charge-discharges, various aspects of performance index can keep preferable.Embodiment 12~14 is lithium
The preparation embodiment of ion battery negative pole nano-cellulose base flexible composite electrode material：Embodiment 12
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 50wt% single-layer graphenes and 20wt% lithium titanates with part, other steps are complete
It is identical.
Embodiment 13
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 40wt% single-layer graphenes and 30wt% lithium titanates with part, other steps are complete
It is identical.
Embodiment 14
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 30wt% single-layer graphenes and 40wt% lithium titanates with part, other steps are complete
It is identical.
The performance test results such as institute of table 8 of the gained nano-cellulose base flexible composite electrode material of above example 12~14
Show：
Table 8
| Embodiment | Modulus of elasticity (Mpa) | Specific capacity (F/g) | Surface resistance (Ω/sq) |
| 12 | 2261.36 | 86.37 | 14.58 |
| 13 | 2381.24 | 94.28 | 23.74 |
| 14 | 2417.68 | 117.53 | 35.62 |
The gained nano-cellulose base flexible composite electrode material of above example 12~14 folds and cycle charge-discharge 1000
The performance test results after secondary are as shown in table 9：
Table 9
It is to be measured in sweep speed under conditions of 10mv/s with the property indices in upper table 8, table 9.
As can be seen from Table 8, on the basis of embodiment 1~5, after embodiment 12~14 adds lithium titanate, wet method
Obtained nano-cellulose base flexible composite electrode material is molded, specific capacity improves much than embodiment 1~5, and this is metatitanic acid
Lithium and the result of the excellent chemical property comprehensive function of graphene, combination electrode material can be effectively improved by adding part lithium titanate
Combination property.
As can be seen from Table 9, the nano-cellulose base flexible composite electrode material that prepared by embodiment 12~14 passes through
After 1000 foldings and 1000 cycle charge-discharges, various aspects of performance index can keep preferable.Embodiment 15~17 is lithium
Ion battery positive pole nanofiber tries the preparation embodiment of base flexible composite electrode material：Embodiment 15
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 50wt% single-layer graphenes and 20wt% LiFePO 4s with part, other steps
It is identical.
Embodiment 16
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 40wt% single-layer graphenes and 30wt% LiFePO 4s with part, other steps
It is identical.
Embodiment 17
A kind of preparation method of the nano-cellulose base flexible composite electrode material of the present embodiment, compared with Example 1, no
It is that raw material is 30wt% nano-celluloses, 30wt% single-layer graphenes and 40wt% LiFePO 4s with part, other steps
It is identical.
The performance test results such as table 10 of the gained nano-cellulose base flexible composite electrode material of above example 15~17
It is shown：
Table 10
| Embodiment | Modulus of elasticity (Mpa) | Specific capacity (F/g) | Surface resistance (Ω/sq) |
| 15 | 2573.84 | 115.38 | 18.27 |
| 16 | 2387.63 | 127.26 | 26.37 |
| 17 | 2476.38 | 101.27 | 45.38 |
The gained nano-cellulose base flexible composite electrode material of above example 15~17 folds and cycle charge-discharge 1000
The performance test results after secondary are as shown in table 11：
Table 11
It is to be measured in sweep speed under conditions of 10mv/s with the property indices in upper table 10, table 11.
As can be seen from Table 10, on the basis of embodiment 1~5, after embodiment 15~17 adds LiFePO 4,
The nano-cellulose base flexible composite electrode material that wet moulding obtains, specific capacity improve much than embodiment 1~5, and this is
LiFePO 4 and the result of the excellent chemical property comprehensive function of graphene, adding part LiFePO 4 can effectively improve
The combination property of combination electrode material.
As can be seen from Table 11, the nano-cellulose base flexible composite electrode material that prepared by embodiment 15~17 passes through
After 1000 foldings and 1000 cycle charge-discharges, various aspects of performance index can keep preferable.
As can be seen from the above results, the nano-cellulose base flexible composite electrode material that prepared by the present invention, dioxy is added
Respective fake capacitance performance can be played by changing manganese and polyphenyl, improve the electrochemistry of ultracapacitor flexible composite electrode material
Can, embodiment 6~8 is better than embodiment 9~11, that is, the flexible composite electrode material chemical property added after manganese dioxide is better than
Add polyaniline；The excellent chemical property of each of which can be played by adding lithium titanate and LiFePO 4, be respectively increased
The chemical property of flexible lithium ion battery both positive and negative polarity electrode material.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of nano-cellulose base flexible composite electrode material, it is characterised in that including following preparation process：
(1) by nano-cellulose, graphene, active material is added or be added without, is added in distilled water and is mixed after mixing
Even, mashing, it is ultrasonically treated, obtains mixed slurry；
(2) mixed slurry obtained by step (1) is manufactured paper with pulp shaping by wet papermaking process, the nano-cellulose is obtained after drying
Base flexible composite electrode material.
2. a kind of preparation method of nano-cellulose base flexible composite electrode material according to claim 1, its feature exist
In：Described nano-cellulose size is 10~100nm, and described graphene refers to single-layer graphene.
3. a kind of preparation method of nano-cellulose base flexible composite electrode material according to claim 1, its feature exist
In：Described active material is at least one of manganese dioxide, polyaniline, aluminium titanates and ferrous phosphate aluminium.
4. a kind of preparation method of nano-cellulose base flexible composite electrode material according to claim 1, its feature exist
In：Described shaping of manufacturing paper with pulp refers to shaping of being manufactured paper with pulp on cylinder mould machine or oblique net paper machine, the quantification of 5~30g/ for shaping of manufacturing paper with pulp
m2, thickness is 10~100 μm.
5. a kind of preparation method of nano-cellulose base flexible composite electrode material according to claim 1, its feature exist
In：The temperature of the drying is 105 DEG C.
A kind of 6. nano-cellulose base flexible composite electrode material, it is characterised in that：By described in any one of Claims 1 to 5
Method be prepared.
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| CN110581267A (en) * | 2019-09-16 | 2019-12-17 | 哈尔滨工业大学 | nano-cellulose-silicon-graphite micron sheet flexible electrode material and preparation method and application thereof |
| CN111710537A (en) * | 2020-06-15 | 2020-09-25 | 浙江理工大学 | Preparation method of cellulose-based hydrogel with high capacitive performance |
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| CN108584934A (en) * | 2018-04-26 | 2018-09-28 | 湖南大学 | A kind of sulfonic functional graphene dispersion system and preparation method thereof |
| CN109742405A (en) * | 2018-12-29 | 2019-05-10 | 中南林业科技大学 | Adjustable flexible electrode material in aperture and the preparation method and application thereof |
| CN109742405B (en) * | 2018-12-29 | 2020-07-10 | 中南林业科技大学 | Aperture-adjustable flexible electrode material and preparation method and application thereof |
| CN109786119A (en) * | 2019-01-23 | 2019-05-21 | 三峡大学 | A kind of method of porous electrode and its conductive treatment |
| CN109786119B (en) * | 2019-01-23 | 2020-01-07 | 三峡大学 | Porous electrode and conductive treatment method thereof |
| CN110581267A (en) * | 2019-09-16 | 2019-12-17 | 哈尔滨工业大学 | nano-cellulose-silicon-graphite micron sheet flexible electrode material and preparation method and application thereof |
| CN110581267B (en) * | 2019-09-16 | 2022-09-13 | 哈尔滨工业大学 | Nano-cellulose-silicon-graphite micron sheet flexible electrode material and preparation method and application thereof |
| CN111710537A (en) * | 2020-06-15 | 2020-09-25 | 浙江理工大学 | Preparation method of cellulose-based hydrogel with high capacitive performance |
| CN111710537B (en) * | 2020-06-15 | 2021-12-03 | 浙江理工大学 | Preparation method of cellulose-based hydrogel with high capacitive performance |
| CN112176771A (en) * | 2020-09-25 | 2021-01-05 | 柔电（武汉）科技有限公司 | Preparation method of lithium-philic carbon nanotube paper and preparation method of composite metal lithium cathode |
| CN112086299A (en) * | 2020-09-30 | 2020-12-15 | 华南理工大学 | Flexible thin film electrode material of super capacitor and preparation method thereof |
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