CN109573997A - A kind of preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material - Google Patents
A kind of preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material Download PDFInfo
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Abstract
The present invention relates to graphene composite material technical field, especially a kind of preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material, comprising the following steps: (1) weigh graphene oxide rGO, copper nitrate CuNO in proportion3With vulcanized sodium Na2S is dissolved in solvent, then solution is transferred in the beaker of sealing, and mixed solution is obtained after stirring；(2) step (1) resulting mixed solution is transferred in hydrothermal reaction kettle, then hydrothermal reaction kettle is placed in baking oven and carries out hydro-thermal reaction, oven temperature is 160 DEG C -280 DEG C；(3) the resulting hydro-thermal reaction product of step (2) is subjected to eccentric cleaning in centrifuge, then place the product in dry in drying box；(4) step (3) resulting product is placed in progress process control heating in tube furnace, final temperature is 600 DEG C -1000 DEG C, after heat preservation, is sintered in the case where argon gas is protective gas, so that it is carbonized, target composite material can be obtained.
Description
Technical field
The present invention relates to graphene composite material technical field, specific field is multiple for a kind of graphene oxide-loaded copper sulfide
The preparation method of condensation material.
Background technique
Graphene is a kind of two-dimentional carbon nanomaterial being made of carbon atom, has excellent physics characteristic, in material
Science, information science, the energy, biological medicine etc. are with a wide range of applications, it is considered to be a kind of future is revolutionary
Material.Graphene is also one of highest material of known strength, but also has good toughness, therefore be to prepare high-strength green wood
The first choice of material.Common graphene composite material has: graphene-nano composition, Graphene polymer composite,
Graphene-carbon-based material composite material and graphene-metal-base composites etc..Graphene has the thermal conductivity of superelevation, addition
In metallic matrix, it can be improved composite materials property simultaneously, improving the thermal conductivity of metal-base composites.
Graphene oxide is the derivative of graphene, it has, and preparation is simple, is easy to get, and has good water-wet behavior,
It is less likely to occur to reunite in aqueous solution.
But it is more complicated for the preparation method of graphene oxide-loaded metal material at present, and energy consumption is higher, this and it is green
The idea of development of the color energy runs in the opposite direction.Based on this, it is simple, environmentally protective graphene oxide-loaded to develop a kind of preparation method
The preparation method for vulcanizing carbon/carbon-copper composite material has greater significance.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of graphene oxide-loaded vulcanization carbon/carbon-copper composite material, to solve
The problems such as preparation method of the prior art is complicated, energy consumption is higher.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material, comprising the following steps:
(1) graphene oxide rGO, copper nitrate CuNO are weighed in proportion3With vulcanized sodium Na2S is dissolved in solvent, then by solution
It is transferred in the beaker of sealing, mixed solution is obtained after stirring；
(2) step (1) resulting mixed solution is transferred in hydrothermal reaction kettle, then hydrothermal reaction kettle is placed in baking oven
Hydro-thermal reaction is carried out, oven temperature is 160 DEG C -280 DEG C；
(3) the resulting hydro-thermal reaction product of step (2) is subjected to eccentric cleaning in centrifuge, then place the product in dry
It is dried in dry case；
(4) step (3) resulting product being placed in tube furnace progress process control heating, final temperature is 600 DEG C-
It 1000 DEG C, after heat preservation, is sintered in the case where argon gas is protective gas, so that it is carbonized, target composite material can be obtained.
Wherein, in the step (1), the mass ratio of graphene oxide, copper nitrate and sodium sulphate is 1:1:1-8:4:1.
Wherein, in the step (1), solvent is dehydrated alcohol or n,N-Dimethylformamide.
Wherein, in the step (1), using magnetic stirrer, stirring rate 350rpm-500rpm.
Wherein, in the step (1), mixing time 6h-8h.
Wherein, in the step (2), reaction time 3h-24h.
Wherein, in the step (3), centrifugal speed 6000rpm-8000rpm, centrifugation number is 8-10 times, is centrifuged molten
Agent is ultrapure water or ethyl alcohol.
Wherein, in the step (3), drying temperature is 40 DEG C -50 DEG C, drying time 12h-24h.
Wherein, in the step (4), tube furnace heating rate is 6 DEG C/min-8 DEG C/min.
Wherein, in the step (4), soaking time 30min-150min.
The pattern of prepared composite material and crystal structure are utilized into scanning electron microscope (SEM) and X-ray diffraction
(XRD) step (4) products therefrom is characterized, it was demonstrated that material prepared is graphene oxide-loaded copper sulfide.
Compared with prior art, the beneficial effects of the present invention are:
(1) composite material prepared by the present invention is rendered as threadiness, has good pattern；
(2) composite wood material prepared by the present invention is mutually with high purity, does not adulterate other hetero atoms；
(3) composite technology prepared by the present invention is simple and environmentally-friendly, and easy to accomplish commercially produces.
Detailed description of the invention
Fig. 1 is the SEM figure of graphene oxide-loaded vulcanization carbon/carbon-copper composite material prepared by embodiment 1；
Fig. 2 is the SEM figure of graphene oxide-loaded vulcanization carbon/carbon-copper composite material prepared by comparative example 1；
Fig. 3 is the SEM figure of graphene oxide-loaded vulcanization carbon/carbon-copper composite material prepared by comparative example 2；
Fig. 4 is the SEM figure of graphene oxide-loaded vulcanization carbon/carbon-copper composite material prepared by comparative example 3；
Fig. 5 is the XRD diagram of graphene oxide-loaded vulcanization carbon/carbon-copper composite material prepared by embodiment 1.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
Graphene oxide-loaded vulcanization carbon/carbon-copper composite material is to realize according to the following steps in present embodiment:
(1) 1g graphene oxide, 1g copper nitrate and 1g vulcanized sodium are weighed to be dissolved in alcohol solvent, then solution is transferred to close
It in the beaker of envelope, is placed on magnetic stirring apparatus and stirs, stirring rate 350rpm obtains mixed solution after stirring 6h；
(2) step (1) resulting mixed solution is transferred in hydrothermal reaction kettle, then hydrothermal reaction kettle is placed in baking oven
Hydro-thermal reaction is carried out, oven temperature is set as 160 DEG C, reaction time 3h；
(3) the resulting hydro-thermal reaction product of step (2) is subjected to eccentric cleaning in centrifuge, centrifugal speed is
6000rpm, centrifugation number are 8 times, and centrifugation solvent is ultrapure water；Then place the product in drying in drying box, drying temperature is
40 DEG C, drying time 12h；
(4) step (3) resulting product is placed in progress process control heating in tube furnace, tube furnace heating rate is 6
DEG C/min, final temperature is 600 DEG C, soaking time 30min, is sintered in the case where argon gas is protective gas, so that it is carbonized
Target composite material is obtained, the SEM figure and XRD diagram of material respectively refer to Fig. 1 and Fig. 5.
Embodiment 2
Graphene oxide-loaded vulcanization carbon/carbon-copper composite material is realized using following steps in present embodiment:
(1) 8g graphene oxide, 1g copper nitrate and 1g vulcanized sodium are weighed to be dissolved in ultrapure water, then solution is transferred to sealing
Beaker in, be placed on magnetic stirring apparatus and stir, stirring rate 400rpm, stir 7h after, obtain mixed solution；
(2) step (1) resulting mixed solution is transferred in hydrothermal reaction kettle, then hydrothermal reaction kettle is placed in baking oven
Hydro-thermal reaction is carried out, oven temperature is set as 200 DEG C, reaction time 10h；
(3) the resulting hydro-thermal reaction product of step (2) is subjected to eccentric cleaning in centrifuge, centrifugal speed is
7000rpm, centrifugation number are 9 times, and centrifugation solvent is ethyl alcohol；Then place the product in being dried in drying box, drying temperature 45
DEG C, drying time 18h；
(4) step (3) resulting product is placed in progress process control heating in tube furnace, tube furnace heating rate is 7
DEG C/min, final temperature is 800 DEG C, soaking time 50min, is sintered in the case where argon gas is protective gas, so that it is carbonized
Obtain target composite material.
Embodiment 3
Graphene oxide-loaded vulcanization carbon/carbon-copper composite material is realized using following steps in present embodiment:
(1) 8g graphene oxide, 4g copper nitrate and 1g vulcanized sodium are weighed to be dissolved in ultrapure water, then solution is transferred to sealing
Beaker in, be placed on magnetic stirring apparatus and stir, stirring rate 500rpm, stir 8h after, obtain mixed solution；
(2) step (1) resulting mixed solution is transferred in hydrothermal reaction kettle, then hydrothermal reaction kettle is placed in baking oven
Hydro-thermal reaction is carried out, oven temperature is set as 280 DEG C, and the reaction time is for 24 hours；
(3) the resulting hydro-thermal reaction product of step (2) is subjected to eccentric cleaning in centrifuge, centrifugal speed is
8000rpm, centrifugation number are 10 times, and centrifugation solvent is ultrapure water or ethyl alcohol；Then it place the product in being dried in drying box, dries
Temperature is 50 DEG C, and drying time is for 24 hours；
(4) step (3) resulting product is placed in progress process control heating in tube furnace, tube furnace heating rate is 8
DEG C/min, final temperature is 1000 DEG C, soaking time 150min, is sintered in the case where argon gas is protective gas, so that it is carbonized, i.e.,
Target composite material can be obtained.
In order to protrude beneficial effects of the present invention, following comparative example test has also been carried out.
Comparative example 1
(1) it weighs 1g copper nitrate and 1g vulcanized sodium is dissolved in alcohol solvent, then solution is transferred in the beaker of sealing, set
In stirring on magnetic stirring apparatus, stirring rate 350rpm obtains mixed solution after stirring 6h；
(2) step (1) resulting mixed solution is transferred in hydrothermal reaction kettle, then hydrothermal reaction kettle is placed in baking oven
Hydro-thermal reaction is carried out, oven temperature is set as 160 DEG C, reaction time 3h；
(3) the resulting hydro-thermal reaction product of step (2) is subjected to eccentric cleaning in centrifuge, centrifugal speed is
6000rpm, centrifugation number are 8 times, and centrifugation solvent is ultrapure water；Then place the product in drying in drying box, drying temperature is
40 DEG C, drying time 12h；
(4) step (3) resulting product is placed in progress process control heating in tube furnace, tube furnace heating rate is 6
DEG C/min, final temperature is 600 DEG C, soaking time 30min, is sintered in the case where argon gas is protective gas, so that it is carbonized
Obtain target composite material.
Graphene is not added in 1 preparation process of comparative example.
Comparative example 2
(1) it weighs 1g graphene oxide and 1g copper nitrate is dissolved in alcohol solvent, then solution is transferred to the beaker of sealing
It is interior, it is placed on magnetic stirring apparatus and stirs, stirring rate 350rpm obtains mixed solution after stirring 6h；
(2) step (1) resulting mixed solution is transferred in hydrothermal reaction kettle, then hydrothermal reaction kettle is placed in baking oven
Hydro-thermal reaction is carried out, oven temperature is set as 160 DEG C, reaction time 3h；
(3) the resulting hydro-thermal reaction product of step (2) is subjected to eccentric cleaning in centrifuge, centrifugal speed is
6000rpm, centrifugation number are 8 times, and centrifugation solvent is ultrapure water；Then place the product in drying in drying box, drying temperature is
40 DEG C, drying time 12h；
(4) step (3) resulting product is placed in progress process control heating in tube furnace, tube furnace heating rate is 6
DEG C/min, final temperature is 600 DEG C, soaking time 30min, is sintered in the case where argon gas is protective gas, so that it is carbonized
Obtain target composite material.
Vulcanized sodium is not added in 2 preparation process of comparative example.
Comparative example 3
(1) it weighs 1g graphene oxide and 1g vulcanized sodium is dissolved in alcohol solvent, then solution is transferred to the beaker of sealing
It is interior, it is placed on magnetic stirring apparatus and stirs, stirring rate 350rpm obtains mixed solution after stirring 6h；
(2) step (1) resulting mixed solution is transferred in hydrothermal reaction kettle, then hydrothermal reaction kettle is placed in baking oven
Hydro-thermal reaction is carried out, oven temperature is set as 160 DEG C, reaction time 3h；
(3) the resulting hydro-thermal reaction product of step (2) is subjected to eccentric cleaning in centrifuge, centrifugal speed is
6000rpm, centrifugation number are 8 times, and centrifugation solvent is ultrapure water；Then place the product in drying in drying box, drying temperature is
40 DEG C, drying time 12h；
(4) step (3) resulting product is placed in progress process control heating in tube furnace, tube furnace heating rate is 6
DEG C/min, final temperature is 600 DEG C, soaking time 30min, is sintered in the case where argon gas is protective gas, so that it is carbonized
Obtain target composite material.
Copper nitrate is not added in 3 preparation process of comparative example.
By Fig. 1-4, comparative example 1-3 is compared with embodiment 1 it can be seen that (1) graphene oxide, copper nitrate and vulcanized sodium three
Person is indispensable for preparing the material；(2) different feeding sequences and feed ratio can all influence to prepare material
Characteristic features.
Comparative example 4
Patent CN108597906A reports a kind of preparation method of fiber/graphene/copper sulfide flexible electrode material, tool
Body are as follows:
Graphene oxide powder is add to deionized water, the graphite oxide that concentration is 1.5mg/L is made in ultrasonic 60min
Alkene suspension.Cotton fabric, in 100 DEG C of processing 2h, is then cleaned up with deionized water with the sodium hydroxide solution of 1mol/L, in
2h is dried in 110 DEG C of drying boxes.Pretreated cotton fabric is impregnated into the graphene oxide suspension prepared, in room temperature
After lower stirring 30min, it is placed in 50 DEG C of vacuum drying ovens and dries 2h, repeated impregnations-drying course 20 times.By cotton/graphite oxide
Alkene compound fabric be immersed in concentration be 0.5mol/L NaBH4 solution in, in room temperature condition stir 12h, then take out spend from
Sub- water cleans 3 times, and in 100 DEG C of drying 2h, reduction obtains cotton/graphene composite material
Preparation process described in this method is complicated, and the drug variety and dosage that use are more, and process costs are high.
Comparative example 5
Northeast Electric Power University, willow, master thesis " preparation of graphene-supported copper sulfide/zinc sulphide composite material and
Photocatalytic Performance Study " give a kind of preparation method of graphene-supported copper sulfide:
When preparing Cu S/rGO composite material using two-step method, stratiform CuS microballoon is prepared using hydro-thermal method first, is then adopted
Cu S/r GO composite material is prepared with ULTRASONIC COMPLEX method.
Experimentation using hydro-thermal method preparation stratiform Cu S/Zn S microballoon is as follows:
(1) it weighs 0.364gC TAB to be placed in 72mL deionized water, its ultrasound to CTAB is completely dispersed, solution clarification
It is transparent；
(2) 0.725g Cu (NO is separately added into solution3)2·3H2O, while magnetic agitation, after making it completely dissolved,
0.685g thiocarbamide is added, continues magnetic agitation to being completely dissolved；
(3) above-mentioned solution is moved in 100m L polytetrafluoroethyllining lining stainless steel cauldron, it is then dry in 150 DEG C of air blast
Heated at constant temperature is for 24 hours in dry case；
(4) after the reaction was completed, it is cooled to room temperature to reaction kettle, by high speed centrifugation, obtains blackish green product, use deionization
Water and ethyl alcohol cleaning removal impurity, are finally dried in vacuo at 50 DEG C, obtain CuS sphere material.
The experimentation for preparing Cu S/r GO composite material using ULTRASONIC COMPLEX method is as follows:
(1) graphene oxide is prepared using improved Hummers method；
(2) the Cu S sphere material and graphene oxide of certain mass are weighed, 60m L deionized water, ultrasonic treatment is added
2h；
(3) it is added a certain amount of hydrazine hydrate in system, the mass ratio of graphite oxide and hydrazine hydrate is 10:8.Then 95
Isothermal reaction 2h in DEG C oil bath；
(4) above-mentioned solution is continued into ultrasound 2h and black product is obtained, with deionized water and second by being centrifuged at a high speed
Alcohol cleaning removal impurity, is dried in vacuo at 50 DEG C.Prepare Cu S/r GO composite material.
This method preparation process is complicated, at high cost, and cannot achieve preparation of industrialization, low yield.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (10)
1. a kind of preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material, which comprises the following steps:
(1) graphene oxide rGO, copper nitrate CuNO are weighed in proportion3With vulcanized sodium Na2S is dissolved in solvent, then solution is shifted
To the beaker of sealing, mixed solution is obtained after stirring；
(2) step (1) resulting mixed solution is transferred in hydrothermal reaction kettle, then hydrothermal reaction kettle is placed in baking oven and is carried out
Hydro-thermal reaction, oven temperature are 160 DEG C -280 DEG C；
(3) the resulting hydro-thermal reaction product of step (2) is subjected to eccentric cleaning in centrifuge, then place the product in drying boxes
Middle drying；
(4) step (3) resulting product is placed in progress process control heating in tube furnace, final temperature is 600 DEG C -1000
DEG C, after heat preservation, it is sintered in the case where argon gas is protective gas, so that it is carbonized, target composite material can be obtained.
2. the preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material according to claim 1, it is characterised in that: institute
It states in step (1), the mass ratio of graphene oxide, copper nitrate and sodium sulphate is 1:1:1-8:4:1.
3. the preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material according to claim 1, it is characterised in that: institute
It states in step (1), solvent is dehydrated alcohol or n,N-Dimethylformamide.
4. the preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material according to claim 1, it is characterised in that: institute
It states in step (1), using magnetic stirrer, stirring rate 350rpm-500rpm.
5. the preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material according to claim 1, it is characterised in that: institute
It states in step (1), mixing time 6h-8h.
6. the preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material according to claim 1, it is characterised in that: institute
It states in step (2), reaction time 3h-24h.
7. the preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material according to claim 1, it is characterised in that: institute
It states in step (3), centrifugal speed 6000rpm-8000rpm, centrifugation number is 8-10 times, and centrifugation solvent is ultrapure water or second
Alcohol.
8. the preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material according to claim 1, it is characterised in that: institute
It states in step (3), drying temperature is 40 DEG C -50 DEG C, drying time 12h-24h.
9. the preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material according to claim 1, it is characterised in that: institute
It states in step (4), tube furnace heating rate is 6 DEG C/min-8 DEG C/min.
10. the preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material according to claim 1, it is characterised in that:
In the step (4), soaking time 30min-150min.
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| CN110841680A (en) * | 2019-11-04 | 2020-02-28 | 淮阴师范学院 | Preparation method of nitrogen and sulfur-doped graphene-CuS composite material |
| CN111943252A (en) * | 2020-08-14 | 2020-11-17 | 武汉理工大学 | CuS/graphene nanocomposite material, preparation method thereof and application thereof in microwave absorption field |
| CN113087545A (en) * | 2021-04-02 | 2021-07-09 | 浙江大学 | Pure inorganic strengthening-moss removing compound agent for protecting weathered stone cultural relics and preparation method thereof |
| CN114180615A (en) * | 2022-01-18 | 2022-03-15 | 天津城建大学 | Preparation method of copper sulfide/graphene oxide composite film |
| CN114242964A (en) * | 2021-11-08 | 2022-03-25 | 南京航空航天大学 | Electrode material for lithium ion battery cathode and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110841680A (en) * | 2019-11-04 | 2020-02-28 | 淮阴师范学院 | Preparation method of nitrogen and sulfur-doped graphene-CuS composite material |
| CN111943252A (en) * | 2020-08-14 | 2020-11-17 | 武汉理工大学 | CuS/graphene nanocomposite material, preparation method thereof and application thereof in microwave absorption field |
| CN111943252B (en) * | 2020-08-14 | 2022-09-02 | 武汉理工大学 | CuS/graphene nanocomposite material, preparation method thereof and application thereof in microwave absorption field |
| CN113087545A (en) * | 2021-04-02 | 2021-07-09 | 浙江大学 | Pure inorganic strengthening-moss removing compound agent for protecting weathered stone cultural relics and preparation method thereof |
| CN113087545B (en) * | 2021-04-02 | 2022-04-26 | 浙江大学 | Pure inorganic strengthening-moss removing compound agent for protecting weathered stone cultural relics and preparation method thereof |
| CN114242964A (en) * | 2021-11-08 | 2022-03-25 | 南京航空航天大学 | Electrode material for lithium ion battery cathode and preparation method thereof |
| CN114180615A (en) * | 2022-01-18 | 2022-03-15 | 天津城建大学 | Preparation method of copper sulfide/graphene oxide composite film |
| CN114180615B (en) * | 2022-01-18 | 2024-09-06 | 天津城建大学 | Preparation method of copper sulfide/graphene oxide composite film |
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