CN109817917A - A kind of three-dimensional globular conductive graphene/Co1-xThe preparation method of S composite material - Google Patents
A kind of three-dimensional globular conductive graphene/Co1-xThe preparation method of S composite material Download PDFInfo
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- Y02E60/10—Energy storage using batteries
Abstract
A kind of three-dimensional globular conductive graphene/Co1‑xThe preparation method of S composite material, the present invention relates to the preparation methods of graphene composite material.It is preparation method complexity, the technical problem at high cost that solve existing three-dimensional globular graphene composite material.This method: graphene oxide dispersion, then ball-milling treatment are prepared with graphite flake；Then CoCl is added into graphene oxide dispersion2·6H2O adds Na after being uniformly dispersed and adjusting pH value2S·9H2O is uniformly dispersed；Mixed liquor is finally subjected to hydro-thermal reaction, obtains three-dimensional globular conductive graphene/Co1‑xS composite material.Hydrogen-bearing alloy electrode is made in material freeze-drying, maximum hydrogen storage capability reaches 2.14wt%, and after circulation 50 times, hydrogen storage ability remains at 76% or more.Simultaneously under the conditions of the discharge current density of 1000mA/g, discharge capability is maintained at 64% or more.It can be used for hydrogen storage battery field.
Description
Technical field
The present invention relates to the preparation methods of graphene composite material.
Background technique
The reserves of hydrogen in nature are extremely abundant, have highest energy matter ratio, cleanliness without any pollution, therefore, Hydrogen Energy are developed
Various countries' reply energy crisis is had become with storage, environmental problem is solved, seeks the important content of the strategy of sustainable development.
Three-dimensional grapheme material is a kind of important structure and function material, the three-dimensional grapheme of different-shape and its compound
Material has potential application value in terms of hydrogen storage, has caused extensive concern.Theoretically, two-dimensional graphene has super
The advantages that high specific surface area, biggish electric charge transfer rate, excellent mechanical strength, but in practical applications due to two dimension
π-π interaction between graphene sheet layer, causes to be easy to happen reunion and stacking between lamella, so that the big discounting of hydrogen storage property
Button.In order to overcome this disadvantage, need to design the pattern and structure of grapheme material.It is well known that three-dimensional globular graphene material
Material has chondritic, and graphene film interlayer is not closely to be arranged between image-stone ink structure is every layer such by Van der Waals force
Together, but the distance between each graphene sheet layer has been above the sphere of action of Van der Waals force, row between layers
Cloth relative loose can effectively overcome graphene stacking and agglomeration traits.Therefore, graphene is made into three-dimensional globular structure is
One of the optimal path of hydrogen storage property is improved through becoming.
Currently, the method that can prepare three-dimensional globular graphene mainly has template auxiliary law, airsetting matrix self-assembly method, You Bao
Aqueous emulsion method.But there is the disadvantages of the device is complicated, and technique is cumbersome, at high cost in existing method.
Summary of the invention
The present invention is to solve above-mentioned existing three-dimensional globular graphene/Co1-xThe preparation method of S composite material is complicated,
Technical problem at high cost, and a kind of three-dimensional globular conductive graphene/Co is provided1-xThe preparation method of S composite material.
Three-dimensional globular conductive graphene/Co of the invention1-xThe preparation method of S composite material, sequentially includes the following steps:
One, using graphite flake as raw material, use Hummer method preparation concentration for 1.25~1.75mg ml-1Graphite oxide
Alkene dispersion liquid I；
Two, ZrO is pressed2The mass ratio of abrading-ball and graphene oxide is (5~8): 1 ratio, by ZrO2Abrading-ball and graphite oxide
Alkene dispersion liquid I, which is packed into, has ZrO2In the ball grinder of liner, hydrazine hydrate is added, high-purity argon gas is filled with, finally consolidates ball grinder
Due in ball mill, ball grinder is cooled to room by 48~60h of ball milling under conditions of drum's speed of rotation is 1050~1100rpm
Wen Hou obtains graphene oxide dispersion II；
Three, CoCl is added into graphene oxide dispersion II2·6H2O is wherein aoxidized in graphene oxide dispersion II
Graphene and CoCl2·6H2The mass ratio of O is 1:(3.5~9.5), 5~10min of ultrasonic disperse, then with 10mol L-1NaOH
The pH value that solution adjusts mixed dispersion liquid II is 13.55~13.85, obtains mixed dispersion liquid III；
Four, Na is added into mixed dispersion liquid III2S·9H2O, wherein Na2S·9H2O and CoCl2·6H2The molar ratio of O is
1:(0.5~0.7), 20~30min of ultrasonic disperse obtains mixed dispersion liquid IV；
Five, mixed dispersion liquid IV is added in water heating kettle, 12~13h is kept the temperature in 160~180 DEG C of baking oven, is obtained
Three-dimensional globular conductive graphene/Co1-xS composite material.
The present invention uses high-energy ball milling assisting alcohol-hydrothermal method, and higher revolving speed enables graphene oxide to be fully stripped into
Few layer graphene oxide, under high speed conditions, the abrading-ball of high speed increases internal energy sharply, and graphene oxide occurs also
Original, but due to the input of high-energy, and few layer of structure is remain, few layer graphene system has biggish surface after ball milling
Can, it provides the foundation for the reunion balling-up of later period graphene.The strong alkaline condition of water-heat process improves the surface tension of solution,
Be conducive to the formation of spherical three-dimensional product, the three-dimensional globular conductive graphene/Co under the debita spissitudo that the present invention limits1-xS is multiple
Condensation material is a kind of hydrogel, and the hydrogen storage property of the three-dimensional globular material greatly improves.By three-dimensional globular conductive graphene/Co1- xAfter the freeze-drying of S compound hydrogel material, it is prepared into hydrogen-bearing alloy electrode, is applied in the energy resource systems such as nickel-metal hydride battery,
Maximum hydrogen storage capability is had excellent performance up to 2.14wt%, electrochemical hydrogen storage, after circulation 50 times, three-dimensional globular graphene/Co1-xS
The hydrogen storage ability of composite material remains at 76% or more.Simultaneously under the conditions of the discharge current density of 1000mA/g, electric discharge
Ability remains at 64% or more.It can be used for hydrogen storage field.Preparation process of the invention is simple, highly-safe, at low cost.
Detailed description of the invention
Fig. 1 is the three-dimensional globular conductive graphene/Co for testing 1 preparation1-xThe photo of S composite material；
Fig. 2 is the three-dimensional globular conductive graphene/Co for testing 1 preparation1-xThe high power stereoscan photograph of S composite material；
Fig. 3 is the three-dimensional globular conductive graphene/Co for testing 1 preparation1-xThe XRD spectra of S composite material；
Fig. 4 is the three-dimensional globular conductive graphene/Co for testing 1 preparation1-xThe cycle performance curve of S composite material；
Fig. 5 is the three-dimensional globular conductive graphene/Co for testing 1 preparation1-xThe high rate performance curve of S composite material；
Fig. 6 is the three-dimensional globular conductive graphene/Co for testing 2 preparations1-xThe photo of S composite material；
Fig. 7 is the three-dimensional globular conductive graphene/Co for testing 2 preparations1-xThe high power stereoscan photograph of S composite material
Fig. 8 is the three-dimensional globular conductive graphene/Co for testing 2 preparations1-xThe XRD spectra of S composite material；
Fig. 9 is the three-dimensional globular conductive graphene/Co for testing 2 preparations1-xThe cycle performance curve of S composite material；
Figure 10 is the three-dimensional globular conductive graphene/Co for testing 2 preparations1-xThe high rate performance curve of S composite material.
Specific embodiment
Specific embodiment 1: three-dimensional globular conductive graphene/Co of present embodiment1-xThe preparation side of S composite material
Method sequentially includes the following steps:
One, using graphite flake as raw material, use Hummer method preparation concentration for 1.25~1.75mg ml-1Graphite oxide
Alkene dispersion liquid I；
Two, ZrO is pressed2The mass ratio of abrading-ball and graphene oxide is (5~8): 1 ratio, by ZrO2Abrading-ball and graphite oxide
Alkene dispersion liquid I, which is packed into, has ZrO2In the ball grinder of liner, hydrazine hydrate is added, high-purity argon gas is filled with, finally consolidates ball grinder
Due in ball mill, ball grinder is cooled to room by 48~60h of ball milling under conditions of drum's speed of rotation is 1050~1100rpm
Wen Hou obtains graphene oxide dispersion II；
Three, CoCl is added into graphene oxide dispersion II2·6H2O is wherein aoxidized in graphene oxide dispersion II
Graphene and CoCl2·6H2The mass ratio of O is 1:(3.5~9.5), 5~10min of ultrasonic disperse, then with 10mol L-1NaOH
The p H value that solution adjusts mixed dispersion liquid II is 13.55~13.85, obtains mixed dispersion liquid III；
Four, Na is added into mixed dispersion liquid III2S·9H2O, wherein Na2S·9H2O and CoCl2·6H2The molar ratio of O is
1:(0.5~0.7), 20~30min of ultrasonic disperse obtains mixed dispersion liquid IV；
Five, mixed dispersion liquid IV is added in water heating kettle, 12~13h is kept the temperature in 160~180 DEG C of baking oven, is obtained
Three-dimensional globular conductive graphene/Co1-xS composite material.
Specific embodiment 2: the present embodiment is different from the first embodiment in that oxidation stone described in step 1
The concentration of black alkene dispersion liquid I is 1.25~1.75mg ml-1；It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that hydrazine hydrate is molten in step 2
The mass percentage concentration of liquid is 2%~4%；The volume ratio of hydrazine hydrate solution and graphene oxide dispersion I is 1:(30~50)；
It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three described in step 2
High-purity argon gas mass percentage concentration >=99.999%；It is other identical as one of specific embodiment one to three.
With following verification experimental verification beneficial effects of the present invention:
Test 1: three-dimensional globular conductive graphene/Co of this test1-xThe preparation method of S composite material, according to the following steps into
Row:
One, to be purchased from the graphite flake of AlfaAesar (China) Chemical Co., Ltd. as raw material, using Hummer method system
Standby concentration is 1.5mg ml-1Graphene oxide dispersion I；
Two, by 0.36g ZrO2Abrading-ball and the graphene oxide dispersion I of 40ml step 1 preparation, which are packed into, has ZrO2Liner
Ball grinder in, add 1.2ml mass percentage concentration be 4% hydrazine hydrate solution, being filled with quality percent purity is
Ball grinder, is finally fixed in ball mill by 99.999% high-purity argon gas, ball under conditions of drum's speed of rotation is 1050rpm
50h is ground, to the end of ball milling, ball grinder is cooled to room temperature, and obtains graphene oxide/carbon nano tube dispersion liquid II；
Three, 0.33 gram of CoCl is added into 40mL graphene oxide dispersion II2·6H2O, ultrasonic disperse 10min, then
With 10mol L-1NaOH solution adjust mixed dispersion liquid II p H value be 13.65, obtain mixed dispersion liquid III；
Four, 0.66 gram of Na is added into mixed dispersion liquid III2S·9H2O, ultrasonic disperse 30min, obtains mixed dispersion liquid
Ⅳ；
Five, mixed dispersion liquid IV is added in water heating kettle, keeps the temperature 12h in 180 DEG C of baking oven, obtained three-dimensional globular and lead
Graphene/Co1-xS composite material, the three-dimensional globular conductive graphene/Co1-xS composite material is a kind of hydrogel.
Fig. 1 is three-dimensional globular conductive graphene/Co prepared by this test 11-xThe photo of S composite material, can from Fig. 1
Out, which is spherical solid spherical structure, a diameter of 14mm, and sphericity is good.
Fig. 2 is three-dimensional globular conductive graphene/Co prepared by this test 11-xThe high power stereoscan photograph of S composite material,
Figure it is seen that the material has spongy internal structure, and load has nano Co of uniform size on graphene platelet1- xS particle.
Fig. 3 is three-dimensional globular conductive graphene/Co prepared by this test 11-xThe XRD spectra of S composite material；It can be with from Fig. 3
Find out, the composite material is by graphene and Co1-xS composition.
Three-dimensional globular conductive graphene/Co prepared by this test 11-xThe freeze-drying of S composite material compound hydrogel material
It is prepared into hydrogen-storage electrode and composition battery after 48 hours, carries out chemical property test, what is obtained arrives cycle performance curve such as Fig. 4
It is shown.From fig. 4, it can be seen that three-dimensional globular conductive graphene/Co1-xThe maximum hydrogen storage capability of S composite material is 2.14wt%,
Electrochemical hydrogen storage is had excellent performance.After circulation 50 times, hydrogen storage ability remains at 76% or more.Fig. 5 is test 1 preparation three
Tie up spherical conductive graphene/Co1-xThe high rate performance curve of S composite material, from fig. 5, it can be seen that in the electric discharge of 1000mA/g
Under current density condition, discharge capability remains at 64% or more.
Test 2: three-dimensional globular conductive graphene/Co of this test1-xThe preparation method of S composite material, according to the following steps into
Row:
One, to be purchased from the graphite flake of AlfaAesar (China) Chemical Co., Ltd. as raw material, using Hummer method system
Standby concentration is 1.7mg ml-1Graphene oxide dispersion I；
Two, by 0.41 gram of ZrO2Abrading-ball and the graphene oxide dispersion I of 40ml step 1 preparation, which are packed into, has ZrO2Liner
Ball grinder in, add 1.2ml mass percentage concentration be 3% hydrazine hydrate solution, being filled with quality percent purity is
Ball grinder, is finally fixed in ball mill by 99.999% high-purity argon gas, ball under conditions of drum's speed of rotation is 1100rpm
50h is ground, to the end of ball milling, ball grinder is cooled to room temperature, and obtains graphene oxide/carbon nano tube dispersion liquid II；
Three, the CoCl of 0.44g is added into 40mL graphene oxide dispersion II2·6H2O, ultrasonic disperse 10min, then use
10mol L-1NaOH solution adjust mixed dispersion liquid II p H value be 13.85, obtain mixed dispersion liquid III；
Four, the Na of 0.73g is added into mixed dispersion liquid III2S·9H2O, ultrasonic disperse 30min, obtains mixed dispersion liquid
Ⅳ；
Five, mixed dispersion liquid IV is added in water heating kettle, keeps the temperature 12h in 180 DEG C of baking oven, obtained three-dimensional globular and lead
Graphene/Co1-xS composite material, the three-dimensional globular conductive graphene/Co1-xS composite material is a kind of hydrogel.
Fig. 6 is three-dimensional globular conductive graphene/Co prepared by this test 21-xThe photo of S composite material, can from Fig. 6
Out, which is spherical solid spherical structure, a diameter of how many 13mm, and sphericity is good.
Fig. 7 is three-dimensional globular conductive graphene/Co prepared by this test 21-xThe high power stereoscan photograph of S composite material,
From figure 7 it can be seen that the material has spongy internal structure, and load has nano Co of uniform size on graphene platelet1- xS particle.
Fig. 8 is three-dimensional globular conductive graphene/Co prepared by this test 21-xThe XRD spectra of S composite material；It can be with from Fig. 8
Find out, the composite material is by graphene and Co1-xS composition.
By this test 2 prepare by three-dimensional globular conductive graphene/Co1-xS compound hydrogel material is freeze-dried 48 hours
After be prepared into hydrogen-storage electrode, form battery, what is obtained is as shown in Figure 9 to cycle performance curve.From fig. 9, it can be seen that three-dimensional globular
Conductive graphene/Co1-xThe maximum hydrogen storage capability of S composite material is 2.20wt%, and electrochemical hydrogen storage is had excellent performance.In circulation 50
After secondary, hydrogen storage ability remains at 76% or more.Obtained high rate performance curve is as shown in Figure 10, from fig. 10 it can be seen that
Under the conditions of the discharge current density of 1000mA/g, discharge capability remains at 64% or more.
Claims (4)
1. a kind of three-dimensional globular conductive graphene/Co1-xThe preparation method of S composite material, it is characterised in that this method presses following step
It is rapid to carry out:
One, using graphite flake as raw material, use Hummer method preparation concentration for 1.25~1.75mg ml-1Graphene oxide point
Dispersion liquid I；
Two, ZrO is pressed2The mass ratio of abrading-ball and graphene oxide is (5~8): 1 ratio, by ZrO2Abrading-ball and graphene oxide point
Dispersion liquid I, which is packed into, has ZrO2In the ball grinder of liner, hydrazine hydrate is added, high-purity argon gas is filled with, is finally fixed on ball grinder
In ball mill, 48~60h of ball milling under conditions of drum's speed of rotation is 1050~1100rpm, after ball grinder is cooled to room temperature,
Obtain graphene oxide dispersion II；
Three, CoCl is added into graphene oxide dispersion II2·6H2O, wherein graphite oxide in graphene oxide dispersion II
Alkene and CoCl2·6H2The mass ratio of O is 1:(3.5~9.5), 5~10min of ultrasonic disperse, then mixed dispersion liquid is adjusted with NaOH
II p H value is 13.55~13.85, obtains mixed dispersion liquid III；
Four, Na is added into mixed dispersion liquid III2S·9H2O, wherein Na2S·9H2O and CoCl2·6H2The molar ratio of O is 1:
(0.5~0.7), 20~30min of ultrasonic disperse obtain mixed dispersion liquid IV；
Five, mixed dispersion liquid IV is added in water heating kettle, 12~13h is kept the temperature in 160~180 DEG C of baking oven, obtains three-dimensional
Spherical conductive graphene/Co1-xS composite material.
2. a kind of three-dimensional globular conductive graphene/Co according to claim 11-xThe preparation method of S composite material, it is special
Sign is that the concentration of graphene oxide dispersion I described in step 1 is 1.45~1.55mg ml-1。
3. a kind of three-dimensional globular conductive graphene/Co according to claim 1 or 21-xThe preparation method of S composite material,
The mass percentage concentration for being characterized in that hydrazine hydrate solution in step 2 is 2%~4%；Hydrazine hydrate solution and graphene oxide disperse
The volume ratio of liquid I is 1:(30~50).
4. a kind of three-dimensional globular conductive graphene/Co according to claim 1 or 21-xThe preparation method of S composite material,
It is characterized in that mass percentage concentration >=99.999% of high-purity argon gas described in step 2.
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| CN105883939A (en) * | 2016-04-07 | 2016-08-24 | 河北科技师范学院 | Preparation method for nickel sulfide/graphene/carbon nano tube/cobalt sulfide three-dimensional composite hydrogen storage material |
| CN105895869A (en) * | 2016-04-07 | 2016-08-24 | 河北科技师范学院 | Preparation method of nickel sulfide/graphene/cobalt sulfide three-dimensional composite hydrogen storage material |
| KR20160119912A (en) * | 2015-04-06 | 2016-10-17 | 울산과학기술원 | Preparing method of graphene oxide dopeded with cobalt disulfide |
| CN108598427A (en) * | 2018-04-26 | 2018-09-28 | 吉林大学 | The method for improving cobalt sulfide charge and discharge cycles ability by coating redox graphene |
| CN108927177A (en) * | 2018-06-06 | 2018-12-04 | 天津大学 | Graphene-supported cobalt disulfide particulate composite, preparation method and its usage |
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- 2019-01-21 CN CN201910054121.7A patent/CN109817917B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20160119912A (en) * | 2015-04-06 | 2016-10-17 | 울산과학기술원 | Preparing method of graphene oxide dopeded with cobalt disulfide |
| CN105883939A (en) * | 2016-04-07 | 2016-08-24 | 河北科技师范学院 | Preparation method for nickel sulfide/graphene/carbon nano tube/cobalt sulfide three-dimensional composite hydrogen storage material |
| CN105895869A (en) * | 2016-04-07 | 2016-08-24 | 河北科技师范学院 | Preparation method of nickel sulfide/graphene/cobalt sulfide three-dimensional composite hydrogen storage material |
| CN108598427A (en) * | 2018-04-26 | 2018-09-28 | 吉林大学 | The method for improving cobalt sulfide charge and discharge cycles ability by coating redox graphene |
| CN108927177A (en) * | 2018-06-06 | 2018-12-04 | 天津大学 | Graphene-supported cobalt disulfide particulate composite, preparation method and its usage |
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