CN109052344A - A kind of preparation method of graphite phase carbon nitride/nickel oxide composite material - Google Patents
A kind of preparation method of graphite phase carbon nitride/nickel oxide composite material Download PDFInfo
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- CN109052344A CN109052344A CN201810815960.1A CN201810815960A CN109052344A CN 109052344 A CN109052344 A CN 109052344A CN 201810815960 A CN201810815960 A CN 201810815960A CN 109052344 A CN109052344 A CN 109052344A
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- composite material
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- carbon nitride
- phase carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The present invention discloses a kind of preparation method of graphite phase carbon nitride/nickel oxide composite material, and the method includes the steps of: (1) soluble divalent nickel salt and graphite phase carbon nitride ultrasonic disperse being obtained mixed liquor in solvent；(2) precipitating reagent is added in step (1) resulting mixed liquor, and stirs evenly, obtain reaction mixture；(3) reaction mixture obtained by step (2) is transferred to ptfe autoclave and carries out hydro-thermal reaction, after the reaction was completed, reaction kettle is cooled to room temperature, reaction mixture is post-processed to obtain sediment, the precipitating after drying obtains graphite phase carbon nitride/nickel oxide composite material through calcining again.This have the advantage that: graphite phase carbon nitride/nickel oxide composite material manufacturing process is simple, mild condition, equipment investment is small, it is with short production cycle, obtained NiO nanoparticle is evenly distributed on lamellar graphite phase carbon nitride, is expected to be used for the related fieldss such as supercapacitor, battery, photocatalysis and piston abrasion-proof coating.
Description
Technical field
The invention belongs to material manufacture and chemical fields, and in particular to a kind of graphite phase carbon nitride/nickel oxide composite material
Preparation method.
Background technique
In recent years, graphite phase carbon nitride (g-C3N4) cause from the fields such as physics, chemistry, material, the energy, environmental protection crowd
The concern of more scholars.g-C3N4Band-gap energy it is relatively narrow, can directly absorbing wavelength be less than 460nm visible light.Due to g-C3N4Structure
Strong covalent bond between the middle nitrogen there are carbon, so that g-C3N4Also there is good chemical stability, thermal stability and unique electronics
Therefore structure has wide practical use in fields such as photocatalytic hydrogen production by water decomposition, organic synthesis, electric energy storage.g-C3N4Surface
Rich in nitrogen-containing functional group, it is capable of providing a large amount of active site, is conducive to form composite material in conjunction with fake capacitance electrode material.
NiO is a kind of typical p-type semiconductor, has hexagonal structure, and crystal form belongs to NaCl type.Nano-nickel oxide is because of surface atom number
The coordination of more and surface atom is unsaturated, a large amount of unsaturated bond and dangling bonds etc. is then formed, to make the table of nano-nickel oxide
Face activity improves；On the other hand, Ni2+With 3d track, there is the tendency preferentially adsorbed to polyelectron oxygen.By nano-nickel oxide with
g-C3N4It combines to form g-C3N4/ NiO composite material is conducive to improve the exposure level of electrolyte and active material, is conducive to
The wettability of electrolyte is improved, to be conducive to improve the specific capacity and cyclical stability of electrode.
Summary of the invention
It is easy to operate the object of the present invention is to provide a kind of simple process, mild condition, the stone suitable for industrialized production
The preparation method of black phase carbon nitride/nickel oxide composite material.
Specific technical solution is as follows:
The present invention provides a kind of preparation method of graphite phase carbon nitride/nickel oxide composite material, and this method includes following step
It is rapid:
(1) soluble divalent nickel salt and graphite phase carbon nitride ultrasonic disperse are obtained into mixed liquor in solvent；
(2) precipitating reagent is added in step (1) resulting mixed liquor, and stirs evenly, obtain reaction mixture；
(3) reaction mixture obtained by step (2) is transferred to ptfe autoclave and carries out hydro-thermal reaction, reaction is completed
Afterwards, reaction kettle is cooled to room temperature, and reaction mixture is post-processed to obtain sediment, the precipitating after drying is obtained through calcining again
Graphite phase carbon nitride/nickel oxide composite material.
Preferred step (1) the of the present invention soluble divalent nickel salt is one of nickel chloride, nickel acetate or nickel nitrate.
Solvent used in preferred step (1) of the present invention is water or ethylene glycol.
Preferred step (2) the of the present invention precipitating reagent is one of urea, ammonium hydroxide or ammonium oxalate.
The temperature of preferred step (3) the of the present invention hydro-thermal reaction is 120~180 DEG C, and the reaction time is 4~12h.
Preferred step (3) the of the present invention post-processing is that the product after reaction is centrifuged, successively with distillation
It must be precipitated after water, ethanol washing separation.
The temperature of preferred step (3) the of the present invention drying precipitate is 60~100 DEG C.
Preferred step (3) the of the present invention calcination temperature is 300~400 DEG C.
The good effect that the present invention has:
A kind of preparation method of graphite phase carbon nitride/nickel oxide composite material set forth in the present invention, the main table of advantage
Now it is following several respects:
1) manufacturing process is simple, is not required to applying surface activating agent and the not effect of template.
2) reaction condition is mild, simple process, with short production cycle, is easy to operation.
3) graphite phase carbon nitride/nickel oxide composite material preparation method consistent appearance prepared by.
Detailed description of the invention
Fig. 1: graphite phase carbon nitride/nickel oxide composite material TEM photo is made for embodiment 1
Specific embodiment
The method of the present invention is explained further with reference to embodiments, is illustrated.
Embodiment 1
Graphite phase carbon nitride/nickel oxide composite material preparation method the following steps are included:
(1) 1mmol nickel nitrate, 40mg g-C are weighed3N4It is scattered in 20mL ethylene glycol, obtains mixed liquor；
(2) it weighs 1mmol ammonium oxalate and is dissolved in 10mL distilled water, step (1) resulting mixed liquor is added in ammonium oxalate solution
In, and stir evenly, ultrasonic 30min obtains reaction mixture；
(3) reaction mixture 50mL obtained by step (2) is transferred to ptfe autoclave and carries out hydro-thermal reaction, reaction temperature
140 DEG C of degree, reaction time 6h is cooled to room temperature, centrifuge separation, and is precipitated with distilled water, ethanol washing, and 60 DEG C of vacuum are deposited in
It is dry, then g-C is obtained through 400 DEG C of calcining 3h3N4/ NiO composite material, TEM photo are as shown in Figure 1.
Embodiment 2
(1) 1mmol nickel nitrate, 40mg g-C are weighed3N4It is scattered in 40mL distilled water, ultrasonic 30min obtains mixed liquor；
(2) it takes 0.25mL ammonium hydroxide to be added in mixed liquor obtained by step (1), and stirs evenly, ultrasonic 30min, must react mixed
Close object；
(3) reaction mixture 50mL obtained by step (2) is transferred to ptfe autoclave and carries out hydro-thermal reaction, reaction temperature
120 DEG C of degree, reaction time 12h is cooled to room temperature, centrifuge separation, and is precipitated with distilled water, ethanol washing, is deposited in 80 DEG C very
Sky is dry, then obtains g-C through 400 DEG C of calcining 3h3N4/ NiO composite material.
3~embodiment of embodiment 6
Each embodiment and embodiment 1 apply that example 2 is essentially identical, and difference is as follows:
Precipitating reagent in embodiment 3 is that 5mmol urea is added, other steps are same as Example 2.
The solvable nickel salt of divalent in embodiment 4 is nickel acetate, other steps are same as Example 1.
The solvable nickel salt of divalent in embodiment 5 is nickel chloride, other steps are same as Example 2.
Hydrothermal temperature in embodiment 6 is 140 DEG C, other steps are same as Example 2.
Although above-described embodiment is not directed to the selection in relation to parameter disclosed full scope, in other implementation
In example, the present invention can realize in the full scope of disclosed related parameter.In addition, the present invention is also not limited to above-mentioned act
Example, those skilled in the art's made variation, increase and decrease or replacement within the essential scope of the present invention, should also belong to
In protection scope of the present invention.
Claims (8)
1. a kind of preparation method of graphite phase carbon nitride/nickel oxide composite material, which is characterized in that this method includes following step
It is rapid:
(1) soluble divalent nickel salt and graphite phase carbon nitride ultrasonic disperse are obtained into mixed liquor in solvent；
(2) precipitating reagent is added in step (1) resulting mixed liquor, and stirs evenly, obtain reaction mixture；
(3) reaction mixture obtained by step (2) is transferred to ptfe autoclave and carries out hydro-thermal reaction, after the reaction was completed, instead
It answers kettle to be cooled to room temperature, reaction mixture is post-processed to obtain sediment, the precipitating after drying obtains graphite through calcining again
Phase carbon nitride/nickel oxide composite material.
2. the preparation method of composite material according to claim 1, which is characterized in that step (1) the soluble nickelous
Salt is one of nickel chloride, nickel acetate or nickel nitrate.
3. the preparation method of composite material according to claim 1, which is characterized in that solvent used in step (1) be water or
Ethylene glycol.
4. the preparation method of composite material according to claim 1, which is characterized in that step (2) precipitating reagent be urea,
One of ammonium hydroxide or ammonium oxalate.
5. the preparation method of composite material according to claim 1, which is characterized in that the temperature of step (3) described hydro-thermal reaction
Degree is 120~180 DEG C, and the reaction time is 4~12h.
6. the preparation method of composite material according to claim 1, which is characterized in that step (3) post-processing is will be anti-
Product after answering is centrifuged, and must precipitate after successively being separated with distilled water, ethanol washing.
7. the preparation method of composite material according to claim 1, which is characterized in that the drying of step (3) described sediment
Temperature is 60~100 DEG C.
8. the preparation method of composite material according to claim 1, which is characterized in that step (3) calcination temperature is 300
~400 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110142059A (en) * | 2019-05-30 | 2019-08-20 | 西北民族大学 | Ni-NiO/g-C3N4The preparation method of nanocomposite |
| CN110350209A (en) * | 2019-07-25 | 2019-10-18 | 河南师范大学 | A kind of preparation method and applications of the NiO/C bifunctional electrocatalyst with core-shell structure |
| CN115121253A (en) * | 2022-06-23 | 2022-09-30 | 四川启睿克科技有限公司 | NiO/g-C based on crystal face effect strategy 3 N 4 Photocatalytic hydrogen production cathode material and preparation method thereof |
| WO2024036756A1 (en) * | 2022-08-19 | 2024-02-22 | 台州学院 | Multifunctional phosphorus and nickel doped graphite-like carbon nitride nanosheet, preparation method therefor, and abs material |
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| CN110142059A (en) * | 2019-05-30 | 2019-08-20 | 西北民族大学 | Ni-NiO/g-C3N4The preparation method of nanocomposite |
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| CN110350209A (en) * | 2019-07-25 | 2019-10-18 | 河南师范大学 | A kind of preparation method and applications of the NiO/C bifunctional electrocatalyst with core-shell structure |
| CN115121253A (en) * | 2022-06-23 | 2022-09-30 | 四川启睿克科技有限公司 | NiO/g-C based on crystal face effect strategy 3 N 4 Photocatalytic hydrogen production cathode material and preparation method thereof |
| CN115121253B (en) * | 2022-06-23 | 2023-06-09 | 四川启睿克科技有限公司 | NiO/g-C based on crystal face effect strategy 3 N 4 Photocatalytic hydrogen production cathode material and preparation method thereof |
| WO2024036756A1 (en) * | 2022-08-19 | 2024-02-22 | 台州学院 | Multifunctional phosphorus and nickel doped graphite-like carbon nitride nanosheet, preparation method therefor, and abs material |
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Application publication date: 20181221 |