CN103407991B - Preparation method of nickel/nickel oxide-decorated nitrogen-doped graphene material - Google Patents
Preparation method of nickel/nickel oxide-decorated nitrogen-doped graphene material Download PDFInfo
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- CN103407991B CN103407991B CN201310289517.2A CN201310289517A CN103407991B CN 103407991 B CN103407991 B CN 103407991B CN 201310289517 A CN201310289517 A CN 201310289517A CN 103407991 B CN103407991 B CN 103407991B
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Abstract
The invention provides a preparation method of a nickel/nickel oxide-decorated nitrogen-doped graphene material. The method comprises the following steps of: evenly dopping nitrogen elements in phene into a graphene slice; distributing nickel/nickel oxide particles on the graphene slice. The nickel/nickel oxide-decorated nitrogen-doped graphene material can be possibly applied to the fields of fuel cells, photocatalysis, biological catalysis, supercapacitors and the like. The nickel/nickel oxide-decorated nitrogen-doped graphene material has the beneficial effects that 1, compared with the pure graphene, the prepared graphene material decorated by nickel, nickel oxide and nitrogen has new properties; 2, a high-temperature heat treatment method is adopted, so that the equipment is simple and the production cost is low; 3, the adopted nickel phthalocyanine can be used for providing a nitrogen source and a nickel source simultaneously, so that the graphene material can be prepared by one step; 4, the graphene material is high in yield, so that the requirement of quantitative production is satisfied.
Description
Technical field
The present invention relates to the preparation method that a kind of nickel/nickel oxide modifies nitrogen-doped graphene material.
Background technology
Graphene is the novel 2D carbon structure of one that the people such as strong K sea nurse (Andre K.Geim) of the peace moral of Univ Manchester UK in 2004 find, because the structure of its uniqueness and physical and chemical performance receive the extensive attention of people.Graphene has that specific surface area is large, conductivity high, has important researching value and application prospect in fields such as fuel cell, ultracapacitor, biocatalysis, lithium ion batteries.
Doping is a kind of method of conventional adjustment Graphene performance, can effectively widen and promote the practical application of grapheme material.Correlative study shows: N doping can change electronic structure and the energy band structure of Graphene, increases the reactive behavior point of graphenic surface, strengthens oxygen reduction catalyst, the biocatalysis performance of Graphene; N doping also can introduce avtive spot on Graphene, contribute to the immobilized of metallic particles, widen application (Haibo Wang, Thandavarayan Maiyalagan, the and Xin Wang at catalytic field, Review on recent progress in nitrogen-dopedgraphene:synthesis, characterization, and its potential applications [J], ACS Catalysis, 2 (2012), 781-794.).Recent research shows: the Graphene that Ni and NiO modifies can catalytic water cracking effectively, improves hydrogen yield; This material is also expected to for fuel cell, lithium ion battery, sensor field (A KAgegnechu et al.Enhanced hydrogen generation by cocatalytic Ni and NiO nanoparticlesloaded on graphene oxide sheets [J], J.Mater.Chem., 22 (2012), 13849-13854.).Therefore, the doping studying Graphene is a significant problem.
Summary of the invention
The technical problem solved
In order to avoid the deficiencies in the prior art part, the present invention proposes the preparation method that a kind of nickel/nickel oxide modifies nitrogen-doped graphene material, and by alkene, nitrogen element Uniform Doped is in graphene film, and nickel/nickel oxide is distributed on graphene film in granular form.This nickel/nickel oxide is modified nitrogen-doped graphene and is expected to for fields such as fuel cell, photochemical catalysis, biocatalysis, ultracapacitors.
Technical scheme
Nickel/nickel oxide modifies a preparation method for nitrogen-doped graphene material, it is characterized in that step is as follows:
The preparation of step 1, graphite oxide: container is positioned in ice-water bath, pours the vitriol oil into; By 3g crystalline graphite powder, 1.5g NaNO
3pour in flask, stir, then cool 3h, make system temperature be 0 DEG C; 9g KMnO is added in mixing solutions
4, stir, period keeps system temperature below 20 DEG C; Container is moved into oil bath pan, after 35 DEG C of constant temperature 2h, adds deionized water, after 10min, add the hydrogen peroxide of dilution, obtain bright yellow solution; Filter reactant, use hydrochloric acid and the distilled water repetitive scrubbing of 10% respectively, suction filtration, dialysis gained sticky solid is close neutral to pH value; Dry, grinding gained solid is graphite oxide;
The dispersion of step 2, graphene oxide: the graphite oxide taking 60 ~ 100mg, measures 300 ~ 500mL dehydrated alcohol, ultrasonic with conventional ultrasound cleanser, disperses 5h with 40kHz, 100W, the alcohol dispersion liquid of configuration graphene oxide.Period keeps temperature to be 25 DEG C;
The compound of step 3, graphene oxide/Nickel Phthalocyanine: take 60 ~ 100mg Nickel Phthalocyanine, pour in the alcohol dispersion liquid of the graphene oxide that step 2 configures, ultrasonic with conventional ultrasound cleanser, with 40kHz, 100W disperses 6h, and ultrasonic period keeps temperature to be 25 DEG C; Then mixing solutions is put into baking oven, 80 DEG C of oven dry, to sample complete drying; Take out beaker, scrape reactant, put into mortar and fully grind, obtain graphene oxide/Nickel Phthalocyanine powder;
Step 4, nickel/nickel oxide modifies the preparation of nitrogen-doped graphene: graphene oxide step 3 obtained/Nickel Phthalocyanine powder pours porcelain boat into, then porcelain boat is loaded silica tube heating zone, and two ends adopt rubber stopper seal; After the rubber plug of jam-pack silica tube two ends, be evacuated to vacuum tightness and be less than 0.10MPa, then pass into argon gas to normal pressure, repeat to vacuumize; In triplicate, ensure that silica tube is interior remaining without obvious oxygen; Continue to pass into argon gas, and with ramp to 800 ~ 1000 DEG C of 10 DEG C/min; By powder 800 ~ 1000 DEG C of annealing 1h in argon gas atmosphere; Period, argon flow amount was 100sccm; After annealing terminates, powered-down, is chilled to room temperature by porcelain boat stove; Stop ventilation, take out porcelain boat, collecting reaction product, obtain nickel/nickel oxide and modify nitrogen-doped graphene material.
Beneficial effect
A kind of nickel that the present invention proposes/nickel oxide modifies the preparation method of nitrogen-doped graphene material, and by black alkene, nitrogen element Uniform Doped is in graphene film, and nickel/nickel oxide is distributed on graphene film in granular form.This nickel/nickel oxide is modified nitrogen-doped graphene and is expected to for fields such as fuel cell, photochemical catalysis, biocatalysis, ultracapacitors.
Beneficial effect of the present invention:
1, prepare a kind of nickel/nickel oxide and modify nitrogen-doped graphene material.Compared with pure Graphene, the co-modified Graphene of nickel, nickel oxide, nitrogen has new character.
2, use high-temperature heat treatment method, equipment is simple, and production cost is low.
3, the Nickel Phthalocyanine adopted can provide nitrogenous source, nickel source simultaneously, realizes the step preparation that nickel/nickel oxide modifies nitrogen-doped graphene material.
4, the productive rate of product is high, can reach the requirement quantizing to produce.
Accompanying drawing explanation
Fig. 1 is thermal treatment unit schematic diagram of the present invention;
Fig. 2 is the transmission electron microscope photo of the nickel/nickel oxide modification nitrogen-doped graphene material prepared by the embodiment of the present invention one;
Fig. 3 is the XPS collection of illustrative plates of the nickel/nickel oxide modification nitrogen-doped graphene material prepared by the embodiment of the present invention one;
Fig. 4 is the XRD figure spectrum of the nickel/nickel oxide modification nitrogen-doped graphene material prepared by the embodiment of the present invention one.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1:
(1) preparation of graphite oxide: be positioned over by flask in ice-water bath, pours the appropriate vitriol oil into; By 3g crystalline graphite powder, 1.5g NaNO
3pour in flask, stir, then cool 3h, make system temperature be 0 DEG C; 9g KMnO is added in mixing solutions
4, stir, period keeps system temperature below 20 DEG C; Flask is moved into oil bath pan, after 35 DEG C of constant temperature 2h, adds deionized water, after 10min, add the hydrogen peroxide of dilution, obtain bright yellow solution; Filter reactant, use hydrochloric acid and the distilled water repetitive scrubbing of 10% respectively, suction filtration, dialysis gained sticky solid is close neutral to pH value; Dry, grinding gained solid, obtains graphite oxide.
(2) dispersion of graphene oxide: take 60mg by the graphite oxide prepared by step 1, measure 500mL dehydrated alcohol, pour in beaker, disperses 5h with conventional ultrasound cleanser ultrasonic (40kHz, 100W), the alcohol dispersion liquid of configuration graphene oxide.Period keeps temperature to be 25 DEG C.
(3) compound of graphene oxide/Nickel Phthalocyanine: take 60mg Nickel Phthalocyanine, pours in the alcohol dispersion liquid of the graphene oxide that step 2 configures, and disperses 6h with conventional ultrasound cleanser ultrasonic (40kHz, 100W).Ultrasonic period keeps temperature to be 25 DEG C.Mixing solutions is put into baking oven, and 80 DEG C of oven dry, to sample complete drying.Take out beaker, scrape sample, put into mortar and fully grind, obtain graphene oxide/Nickel Phthalocyanine powder.
(4) nickel/nickel oxide modifies the preparation of nitrogen-doped graphene: graphene oxide step 3 obtained/Nickel Phthalocyanine powder pours porcelain boat into, then porcelain boat is loaded silica tube heating zone, and two ends adopt rubber stopper seal.After the rubber plug of jam-pack silica tube two ends, be evacuated to vacuum tightness and be less than 0.10MPa, then pass into argon gas to normal pressure, repeat to vacuumize.In triplicate, ensure that silica tube is interior remaining without obvious oxygen.Continue to pass into argon gas, and with the ramp to 1000 DEG C of 10 DEG C/min.Powder 1000C thermal treatment 1h(experimental installation in argon gas atmosphere is shown in Fig. 1).Period, argon flow amount was 100sccm.After annealing terminates, powered-down, is chilled to room temperature by porcelain boat stove.Stop ventilation, take out porcelain boat, collecting reaction product, obtain nickel/nickel oxide and modify nitrogen-doped graphene material.
This nickel/nickel oxide modifies the transmission electron microscope photo of nitrogen-doped graphene as shown in Figure 2.Can see, metallic particles is not of uniform size, and load is on graphene film.Fig. 3 is the XPS collection of illustrative plates of its correspondence.As seen from the figure, compared to graphene oxide, in product, there is N, Ni, show the successful doping of N, Ni.In Fig. 3, O peak intensity falls sharply, and shows that the graphene oxide in raw material is successfully reduced.XPS quantitative analysis shows, in product, N content is 2.54at.%, Ni content is 0.25at.%.Fig. 4 is the XRD figure spectrum of its correspondence.In figure, DEG C peak (2 θ=26.1 °) come from Graphene; Ni and NiO peak comes from Nickel Phthalocyanine.In figure Ni 44.36 °, three peaks, 51.71 °, 76.09 ° correspond respectively to (111), (200), (220) three crystal faces.43.28 °, three peaks of NiO, 51.75 °, 76.09 ° correspond respectively to (012), (003), (110) three crystal faces.
Embodiment 2:
(1) preparation of graphite oxide: be positioned over by flask in ice-water bath, pours the appropriate vitriol oil into; By 3g crystalline graphite powder, 1.5g NaNO
3pour in flask, stir, then cool 3h, make system temperature be 0 DEG C; 9g KMnO is added in mixing solutions
4, stir, period keeps system temperature below 20 DEG C; Flask is moved into oil bath pan, after 35 DEG C of constant temperature 2h, adds deionized water, after 10min, add the hydrogen peroxide of dilution, obtain bright yellow solution; Filter reactant, use hydrochloric acid and the distilled water repetitive scrubbing of 10% respectively, suction filtration, dialysis gained sticky solid is close neutral to pH value; Dry, grinding gained solid, obtains graphite oxide.
(2) dispersion of graphene oxide: take 20mg by the graphite oxide prepared by step 1, measure 300mL dehydrated alcohol, pour in beaker, disperses 5h with conventional ultrasound cleanser ultrasonic (40kHz, 100W), the alcohol dispersion liquid of configuration graphene oxide.Period keeps temperature to be 25 DEG C.
(3) compound of graphene oxide/Nickel Phthalocyanine: take 100mg Nickel Phthalocyanine, pours in the alcohol dispersion liquid of the graphene oxide that step 2 configures, and disperses 6h with conventional ultrasound cleanser ultrasonic (40kHz, 100W).Ultrasonic period keeps temperature to be 25 DEG C.Mixing solutions is put into baking oven, and 80 DEG C of oven dry, to sample complete drying.Take out beaker, scrape sample, put into mortar and fully grind, obtain graphene oxide/Nickel Phthalocyanine powder.
(4) nickel/nickel oxide modifies the preparation of nitrogen-doped graphene: graphene oxide step 3 obtained/Nickel Phthalocyanine powder pours porcelain boat into, then porcelain boat is loaded silica tube heating zone, and two ends adopt rubber stopper seal.After the rubber plug of jam-pack silica tube two ends, be evacuated to vacuum tightness and be less than 0.10MPa, then pass into argon gas to normal pressure, repeat to vacuumize.In triplicate, ensure that silica tube is interior remaining without obvious oxygen.Continue to pass into argon gas, and with the ramp to 1000 DEG C of 10 DEG C/min.Powder 1000 DEG C of thermal treatment 1h(experimental installations in argon gas atmosphere are shown in Fig. 1).Period, argon flow amount was 100sccm.After annealing terminates, powered-down, is chilled to room temperature by porcelain boat stove.Stop ventilation, take out porcelain boat, collecting reaction product, nickel/nickel oxide can be obtained and modify nitrogen-doped graphene material.
Embodiment 3:
(1) preparation of graphite oxide: be positioned over by flask in ice-water bath, pours the appropriate vitriol oil into; By 3g crystalline graphite powder, 1.5g NaNO
3pour in flask, stir, then cool 3h, make system temperature be 0 DEG C; 9g KMnO is added in mixing solutions
4, stir, period keeps system temperature below 20 DEG C; Flask is moved into oil bath pan, after 35 DEG C of constant temperature 2h, adds deionized water, after 10min, add the hydrogen peroxide of dilution, obtain bright yellow solution; Filter reactant, use hydrochloric acid and the distilled water repetitive scrubbing of 10% respectively, suction filtration, dialysis gained sticky solid is close neutral to pH value; Dry, grinding gained solid, obtains graphite oxide.
(2) dispersion of graphene oxide: take 60mg by the graphite oxide prepared by step 1, measure 500mL dehydrated alcohol, pour in beaker, disperses 5h with conventional ultrasound cleanser ultrasonic (40kHz, 100W), the alcohol dispersion liquid of configuration graphene oxide.Period keeps temperature to be 25 DEG C.
(3) compound of graphene oxide/Nickel Phthalocyanine: take 60mg Nickel Phthalocyanine, pours in the alcohol dispersion liquid of the graphene oxide that step 2 configures, and disperses 6h with conventional ultrasound cleanser ultrasonic (40kHz, 100W).Ultrasonic period keeps temperature to be 25 DEG C.Mixing solutions is put into baking oven, and 80 DEG C of oven dry, to sample complete drying.Take out beaker, scrape sample, put into mortar and fully grind, obtain graphene oxide/Nickel Phthalocyanine powder.
(4) nickel/nickel oxide modifies the preparation of nitrogen-doped graphene: graphene oxide step 3 obtained/Nickel Phthalocyanine powder pours porcelain boat into, then porcelain boat is loaded silica tube heating zone, and two ends adopt rubber stopper seal.After the rubber plug of jam-pack silica tube two ends, be evacuated to vacuum tightness and be less than 0.10MPa, then pass into argon gas to normal pressure, repeat to vacuumize.In triplicate, ensure that silica tube is interior remaining without obvious oxygen.Continue to pass into argon gas, and with the ramp to 1000 DEG C of 10 DEG C/min.Powder 800 DEG C of thermal treatment 1h(experimental installations in argon gas atmosphere are shown in Fig. 1).Period, argon flow amount was 100sccm.After annealing terminates, powered-down, is chilled to room temperature by porcelain boat stove.Stop ventilation, take out porcelain boat, collecting reaction product, nickel/nickel oxide can be obtained and modify nitrogen-doped graphene material.
Claims (1)
1. nickel/nickel oxide modifies a preparation method for nitrogen-doped graphene material, it is characterized in that step is as follows:
The preparation of step 1, graphite oxide: container is positioned in ice-water bath, pours the vitriol oil into; By 3g crystalline graphite powder, 1.5g NaNO
3pour in flask, stir, then cool 3h, make system temperature be 0 DEG C; 9g KMnO is added in mixing solutions
4, stir, period keeps system temperature below 20 DEG C; Container is moved into oil bath pan, after 35 DEG C of constant temperature 2h, adds deionized water, after 10min, add the hydrogen peroxide of dilution, obtain bright yellow solution; Filter reactant, use hydrochloric acid and the distilled water repetitive scrubbing of 10% respectively, suction filtration, dialysis gained sticky solid is close neutral to pH value; Dry, grinding gained solid is graphite oxide;
The dispersion of step 2, graphene oxide: the graphite oxide taking 60 ~ 100mg, measures 300 ~ 500mL dehydrated alcohol, ultrasonic with conventional ultrasound cleanser, with 40kHz, 100W disperses 5h, the alcohol dispersion liquid of configuration graphene oxide, and period keeps temperature to be 25 DEG C;
The compound of step 3, graphene oxide/Nickel Phthalocyanine: take 60 ~ 100mg Nickel Phthalocyanine, pour in the alcohol dispersion liquid of the graphene oxide that step 2 configures, ultrasonic with conventional ultrasound cleanser, with 40kHz, 100W disperses 6h, and ultrasonic period keeps temperature to be 25 DEG C; Then mixing solutions is put into baking oven, 80 DEG C of oven dry, to sample complete drying; Take out beaker, scrape reactant, put into mortar and fully grind, obtain graphene oxide/Nickel Phthalocyanine powder;
Step 4, nickel/nickel oxide modifies the preparation of nitrogen-doped graphene: graphene oxide step 3 obtained/Nickel Phthalocyanine powder pours porcelain boat into, then porcelain boat is loaded silica tube heating zone, and two ends adopt rubber stopper seal; After the rubber plug of jam-pack silica tube two ends, be evacuated to vacuum tightness and be less than 0.10MPa, then pass into argon gas to normal pressure, repeat to vacuumize; In triplicate, ensure that silica tube is interior remaining without obvious oxygen; Continue to pass into argon gas, and with ramp to 800 ~ 1000 DEG C of 10 DEG C/min; By powder 800 ~ 1000 DEG C of annealing 1h in argon gas atmosphere; Period, argon flow amount was 100sccm; After annealing terminates, powered-down, is chilled to room temperature by porcelain boat stove; Stop ventilation, take out porcelain boat, collecting reaction product, obtain nickel/nickel oxide and modify nitrogen-doped graphene material.
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| CN103871755A (en) * | 2014-03-05 | 2014-06-18 | 南京理工大学 | N-doped graphene/nickel ferrite nanometer compound material and preparation thereof |
| CN104449239A (en) * | 2014-12-18 | 2015-03-25 | 四川环碳科技有限公司 | Nitrogen-doped graphene composited electromagnetic shielding type electricity conductive primer and preparation method thereof |
| CN105110321A (en) * | 2015-07-29 | 2015-12-02 | 浙江工业大学 | Preparation method for nano-pores on surface of graphene by metal phthalocyanine and its alloy precursor |
| CN106158418B (en) * | 2016-07-14 | 2019-02-05 | 江苏大学 | A kind of preparation method of NiO/ nitrogen-doped graphene composite nano-electrode material |
| CN106944066A (en) * | 2017-03-30 | 2017-07-14 | 常州大学 | A kind of preparation method of hud typed nickel oxide/nickel photochemical catalyst |
| CN109529931B (en) * | 2018-11-16 | 2021-09-28 | 中北大学 | Graphene oxide covalent immobilized metal phthalocyanine catalyst and preparation method and application thereof |
| CN110400935A (en) * | 2019-07-30 | 2019-11-01 | 南京汉尔斯生物科技有限公司 | A kind of preparation method and fuel cell electrode of fuel cell nano-electrode material |
| CN115368801A (en) * | 2021-05-18 | 2022-11-22 | 江苏科辉环境科技有限公司 | Magnetized graphene coating and preparation method thereof |
| CN113550069B (en) * | 2021-08-04 | 2022-10-14 | 安徽锦鼎织造有限公司 | Preparation process of terahertz hot-air cotton |
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| CN102757029B (en) * | 2011-04-26 | 2014-11-05 | 海洋王照明科技股份有限公司 | Nitrogen doped graphene material and preparation method thereof |
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