CN105935777B - A method of preparing graphene/nanometer nickel composite material - Google Patents
A method of preparing graphene/nanometer nickel composite material Download PDFInfo
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- CN105935777B CN105935777B CN201610266045.2A CN201610266045A CN105935777B CN 105935777 B CN105935777 B CN 105935777B CN 201610266045 A CN201610266045 A CN 201610266045A CN 105935777 B CN105935777 B CN 105935777B
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- composite material
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The present invention relates to a kind of methods for preparing graphene/nanometer nickel composite material comprising following processing step: 1), glucose and nickel nitrate being mixed, ground in the agate mortar；2), sodium chloride and potassium chloride are mixed, through ball mill ball milling；3), by step 1) and 2) obtained in material be uniformly mixed, and the pre-heat treatment；4), the mixing material after the pre-heat treatment is placed in rectangular porcelain boat, porcelain boat is placed in tube furnace, inert gas shielding is passed through, is calcined under certain heating rate；5) isothermal holding, is carried out after calcining；6) it, under inert gas protection, is naturally cooling to room temperature, takes out sample；7) gained mixture is cleaned with deionized water, and product is obtained by vacuum filtration.The present invention can prepare graphene/nanometer nickel composite material by the method for one-step synthesis, and primary raw material is glucose, thus have the characteristics that low cost, can large-scale application, be a kind of novel electromagnetic wave absorbent material.
Description
[technical field]
The present invention relates to a kind of preparation methods of composite material, and in particular to a kind of to prepare graphene/nanometer nickel composite wood
The method of material, belongs to technical field of nano material.
[background technique]
With the fast development of electromagnetic wave technology, while in addition to bringing convenient, biggish electromagnetism is also brought
Radiation pollution, slowly development is a new subject to anti-electromagnetic radiation, increasingly obtains the attention of people, researches and develops to electromagnetism
The new material of wave height absorptivity is expected to solve this problem.Traditional absorbing material is using ferrite as main representative, because it has
There is excellent flux loss performance, with the continuous improvement of science and technology and people's life, the absorbing property of single Ferrite Material is
It increasingly cannot meet the needs, the composite wave-suction material of Development of Novel is a trend, is researched and developed lighter, thinner, wider, stronger
Novel wave-absorbing material be current scientific worker's target.
Graphene is a kind of material with excellent mechanics, electricity, both thermally and chemically performance, is deposited in photoelectric display, energy
The fields such as storage have important application, and graphene film edge has functional group abundant, can introduce defect polarization and electronics relaxes
Henan polarization is a kind of excellent absorbing material.Graphene and metal, metal oxide, nonmetal oxide and macromolecule material
The composite material exhibits of material go out excellent electro-magnetic wave absorption ability, especially compound with metallic nickel, the suction because of graphene to wave
Receipts are usually located at high frequency region, and graphene/nickel composite material can effectively widen the absorption bands of electromagnetic wave.Graphene/nickel is compound
The loss of electromagnetic wave can be not only greatly improved in material, be also beneficial to the impedance matching of composite material, the presence of nickel particles is also
Help prevent graphene because Van der Waals adsorption power is reunited, forms stable three-dimensional structure.
And oxidation stone first is synthesized in Hummers method mostly to the synthetic method of graphene/nanometer nickel composite material at present
Black alkene (GO), then graphite oxide is reduced to graphene (RGO), metallic Ni particles are loaded to by graphene by the methods of hydro-thermal
In lamellar structure, complex steps and yield is lower are unsuitable for the large-scale application of the material.
Therefore, in order to solve the above technical problems, preparing graphene/nanometer nickel composite wood it is necessory to provide a kind of innovation
The method of material, to overcome the defect in the prior art.
[summary of the invention]
To solve the above problems, the purpose of the present invention is to provide a kind of extensive, low costs to prepare graphene/nanometer nickel
The method of composite material.
To achieve the above object, the technical scheme adopted by the invention is as follows: a kind of graphene/nanometer nickel composite material of preparing
Method uses one-step synthesis, comprises the technical steps that:
1), glucose and nickel nitrate are mixed, ground in the agate mortar；
2), sodium chloride and potassium chloride are mixed, through ball mill ball milling；
3), by step 1) and 2) obtained in material be uniformly mixed, and the pre-heat treatment；
4), the mixing material after the pre-heat treatment is placed in rectangular porcelain boat, porcelain boat is placed in the middle position of tube furnace,
It is passed through inert gas shielding, is calcined under certain heating rate；
5) isothermal holding, is carried out after calcining；
6) it, under inert gas protection, is naturally cooling to room temperature, takes out sample；
7) gained mixture is cleaned with deionized water, and product is obtained by vacuum filtration.
The method for preparing graphene/nanometer nickel composite material of the invention is further are as follows: in step 1), the glucose and
The mass ratio of nickel nitrate is (1-16): 1.
The method for preparing graphene/nanometer nickel composite material of the invention is further are as follows: in step 2, the sodium chloride and
The mass ratio of potassium chloride is (1-3): 1.
The method for preparing graphene/nanometer nickel composite material of the invention is further are as follows: in step 3), the temperature of the pre-heat treatment
Degree is 80 DEG C -200 DEG C.
The method for preparing graphene/nanometer nickel composite material of the invention is further are as follows: in step 4), heating rate 5
DEG C -30 DEG C/min；Calcination temperature is 950 DEG C -1300 DEG C；The inert gas is nitrogen.
The method for preparing graphene/nanometer nickel composite material of the invention is further are as follows: in step 5), the soaking time
For 30min-60min.
The method for preparing graphene/nanometer nickel composite material of the invention is further are as follows: in step 6), the dilute hydrochloric acid
Concentration is 0.5%.
The method for preparing graphene/nanometer nickel composite material of the invention is further are as follows: in step 1), glucose and nitric acid
It needs that ammonium chloride is added in the mixture of nickel, the mass ratio of the glucose and ammonium chloride is 4:5.
The method for preparing graphene/nanometer nickel composite material of the invention is also are as follows: in step 1), glucose 0.1g, and nitric acid
Nickel 0.1g grinds 50min；In step 2, sodium chloride 11.4g and potassium chloride 2.8g, ball milling 50min；In step 3), at 150 DEG C
The pre-heat treatment 20h；In step 4), 1000 DEG C are warming up to, heating rate is 20 DEG C/min；In step 5), 40min is kept the temperature.
Compared with prior art, the invention has the following beneficial effects: the present invention can pass through the method system of one-step synthesis
Standby graphene/nanometer nickel composite material, primary raw material is glucose, thus have the characteristics that it is inexpensive, can large-scale application, be
A kind of novel electromagnetic wave absorbent material.
[Detailed description of the invention]
Fig. 1 is the X ray diffracting spectrum (XRD) of sample obtained by the present invention.
Fig. 2 is field emission scanning electron microscope (SEM) figure of present invention gained sample.
[specific embodiment]
Embodiment 1:
One, raw material are prefabricated
0.8g glucose is weighed, 0.05g nickel nitrate after being sufficiently mixed in glove box, is placed in agate mortar and grinds
30min obtains mixture A；11.5g sodium chloride and 11.5g potassium chloride are weighed, to be placed in ball milling in ball mill after being sufficiently mixed
30min obtains mixture B；Mixture A and B are mixed, are placed in rectangular porcelain boat, total mixture amount is no more than porcelain boat total amount
2/3rds.
Two, pretreatment
Mixture obtained in step 1 is placed in a vacuum drying oven, is heat-treated 10 at 80 DEG C；
Three, solid phase reaction
Gained mixture in step 2 is placed among tube furnace boiler tube, nitrogen protection is passed through, is warming up to 950 DEG C, heating
Rate is 5 DEG C/min, after reaching target temperature, keeps the temperature 30min, and cooled to room temperature is taken out.
Four, product washs
Porcelain boat product in step 3 is taken out, is placed in 500ml beaker, deionized water is added, 30min is stirred by ultrasonic, adopts
It is filtered by vacuum with the filter membrane of 0.5M, deionized water is added again, wash repeatedly step, washed 3-5 times altogether.Products therefrom is set
It is dried for 24 hours in air dry oven.
Embodiment 2:
One, raw material are prefabricated
0.1g glucose is weighed, 0.1g nickel nitrate after being sufficiently mixed in glove box, is placed in agate mortar and grinds
50min obtains mixture A；11.4g sodium chloride and 2.8g potassium chloride are weighed, to be placed in ball milling in ball mill after being sufficiently mixed
50min obtains mixture B；Mixture A and B are mixed, are placed in rectangular porcelain boat, total mixture amount is no more than porcelain boat total amount
2/3rds.
Two, pretreatment
Mixture obtained in step 1 is placed in a vacuum drying oven, after 150 DEG C of heat treatment 20h；
Three, solid phase reaction
Gained mixture in step 2 is placed among tube furnace boiler tube, nitrogen protection is passed through, is warming up to 1000 DEG C, heating
Rate is 20 DEG C/min, after reaching target temperature, keeps the temperature 40min, and cooled to room temperature is taken out.
Four, product washs
Porcelain boat product in step 3 is taken out, is placed in 500ml beaker, deionized water is added, 30min is stirred by ultrasonic, adopts
It is filtered by vacuum with the filter membrane of 0.5M, deionized water is added again, wash repeatedly step, washed 3-5 times altogether.Products therefrom is set
It is dried for 24 hours in air dry oven.
Embodiment 3:
One, raw material are prefabricated
0.4g glucose, the ammonium chloride of 0.5g are weighed, 0.05g nickel nitrate after being sufficiently mixed in glove box, is placed in agate
60min is ground in mortar, obtains mixture A；13.5g sodium chloride and 11.5g potassium chloride are weighed, to be placed in ball milling after being sufficiently mixed
Ball milling 60min in machine obtains mixture B；Mixture A and B are mixed, are placed in rectangular porcelain boat, total mixture amount is no more than porcelain
2/3rds of boat total amount.
Two, pretreatment
Mixture obtained in step 1 is placed in a vacuum drying oven, after 200 DEG C of heat treatment 30h, is down to room naturally
It is taken out after temperature；
Three, solid phase reaction
Gained mixture in step 2 is placed among tube furnace boiler tube, nitrogen protection is passed through, is warming up to 1300 DEG C, heating
Rate is 30 DEG C/min, after reaching target temperature, keeps the temperature 60min, and cooled to room temperature is taken out.
Four, product washs
Porcelain boat product in step 3 is taken out, is placed in 500ml beaker, deionized water is added, 30min is stirred by ultrasonic, adopts
It is filtered by vacuum with the filter membrane of 0.5M, deionized water is added again, wash repeatedly step, washed 3-5 times altogether.Products therefrom is set
It is dried for 24 hours in air dry oven.
It is referred to shown in Figure of description 1 and attached drawing 2 using the specific material characterization of sample obtained by technique of the invention.
Above specific embodiment is only the preferred embodiment of this creation, all in this wound not to limit this creation
Any modification, equivalent substitution, improvement and etc. done within the spirit and principle of work, should be included in this creation protection scope it
It is interior.
Claims (9)
1. a kind of method for preparing graphene/nanometer nickel composite material, it is characterised in that: it uses one-step synthesis, including such as
Lower processing step:
1), glucose and nickel nitrate are mixed, ground in the agate mortar；
2), sodium chloride and potassium chloride are mixed, through ball mill ball milling；
3), by step 1) and 2) obtained in material be uniformly mixed, and the pre-heat treatment；
4), the mixing material after the pre-heat treatment is placed in rectangular porcelain boat, porcelain boat is placed in the middle position of tube furnace, is passed through
Inert gas shielding is calcined under certain heating rate；
5) isothermal holding, is carried out after calcining；
6) it, under inert gas protection, is naturally cooling to room temperature, takes out sample；
7) gained mixture is cleaned with deionized water, and product is obtained by vacuum filtration.
2. the method for preparing graphene/nanometer nickel composite material as described in claim 1, it is characterised in that: in step 1), institute
The mass ratio for stating glucose and nickel nitrate is (1-16): 1.
3. the method for preparing graphene/nanometer nickel composite material as described in claim 1, it is characterised in that: in step 2, institute
The mass ratio for stating sodium chloride and potassium chloride is (1-3): 1.
4. the method for preparing graphene/nanometer nickel composite material as described in claim 1, it is characterised in that: in step 3), in advance
The temperature of heat treatment is 80 DEG C -200 DEG C.
5. the method for preparing graphene/nanometer nickel composite material as described in claim 1, it is characterised in that: in step 4), rise
Warm rate is 5 DEG C -30 DEG C/min；Calcination temperature is 950 DEG C -1300 DEG C；The inert gas is nitrogen.
6. the method for preparing graphene/nanometer nickel composite material as described in claim 1, it is characterised in that: in step 5), institute
Stating soaking time is 30min-60min.
7. the method for preparing graphene/nanometer nickel composite material as described in claim 1, it is characterised in that:, will in step 7)
Mixture is placed in a beaker, and deionized water is added, and 30min is stirred by ultrasonic, is filtered by vacuum using filter membrane, washes repeatedly step
3-5 times；Products therefrom is placed in air dry oven and dries for 24 hours.
8. the method for preparing graphene/nanometer nickel composite material as described in claim 1, it is characterised in that: in step 1), Portugal
It needs that ammonium chloride is added in the mixture of grape sugar and nickel nitrate, the mass ratio of the glucose and ammonium chloride is 4:5.
9. the method for preparing graphene/nanometer nickel composite material as described in claim 1, it is characterised in that: in step 1), Portugal
Grape sugar 0.1g, nickel nitrate 0.1g grind 50min；In step 2, sodium chloride 11.4g and potassium chloride 2.8g, ball milling 50min；Step
3) in, in 150 DEG C of the pre-heat treatment 20h；In step 4), 1000 DEG C are warming up to, heating rate is 20 DEG C/min；In step 5), protect
Warm 40min.
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| CN109305913B (en) * | 2017-07-28 | 2022-03-11 | 中国石油化工股份有限公司 | Synthesis method of aniline compound |
| CN113677177B (en) * | 2021-08-12 | 2023-11-21 | 广西大学 | Preparation method of graphene-based metal composite material and wave absorbing application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992308A (en) * | 2012-11-21 | 2013-03-27 | 复旦大学 | Graphene with high specific capacitance and preparation method thereof |
| CN103715430A (en) * | 2013-12-23 | 2014-04-09 | 天津大学 | Three-dimensional graphene reticular structure loaded carbon-coated tin nanometer material as well as preparation method and application thereof |
| CN104876217A (en) * | 2015-06-01 | 2015-09-02 | 北京理工大学 | Graphene preparation method |
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| TW201515994A (en) * | 2013-10-28 | 2015-05-01 | Enerage Inc | Nano-graphene hollow particles and manufacturing method thereof |
| US10407774B2 (en) * | 2014-04-17 | 2019-09-10 | Research & Business Foundation Sungkyunkwan University | Metal-containing graphene hybrid composite, and preparing method of the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992308A (en) * | 2012-11-21 | 2013-03-27 | 复旦大学 | Graphene with high specific capacitance and preparation method thereof |
| CN103715430A (en) * | 2013-12-23 | 2014-04-09 | 天津大学 | Three-dimensional graphene reticular structure loaded carbon-coated tin nanometer material as well as preparation method and application thereof |
| CN104876217A (en) * | 2015-06-01 | 2015-09-02 | 北京理工大学 | Graphene preparation method |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis of Monolayer-Patched Graphene from Glucose;Xin-Hao Li et al.;《Angew. Chem. Int. Ed.》;20120917;第51卷(第38期);第9689-9692页 |
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