Preparation method of graphene supported ferriferrous oxide nanocomposite

A nano-composite material, ferric oxide technology, applied in chemical instruments and methods, nanotechnology, nanotechnology and other directions, can solve the problems of difficult calcination and decomposition of iron salts, reduce the difficulty of operation, loss of iron ions, etc. Absorption and other properties, good bonding, good crystallinity

Inactive Publication Date: 2012-09-12
TIANJIN UNIV
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  • Application Information

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Problems solved by technology

[0007] The "CN201110207639.3" patent proposes to obtain a composite material of graphene-loaded ferric oxide by annealing. The method is mainly to combine graphene with Fe(NO) 3 9H 2 O was dissolved in water, and the precipitate was obtained by centrifugation. After washing with ethanol and deionized water, it was annealed at 350 ° C for 2 h to obtain a graphene-loaded ferric oxide composite material. This method uses a simple and easy calcination method instead of the above The two methods reduce the difficulty of operation and reduce the parameters of the reaction, making the reaction more stable and controllable. However, the disadvantages of this method are: ① Since the raw material iron salts are all soluble in water, the centrifugation process It is inevitable to cause a large loss of iron ions in the calcination process; ② There is no reducing atmosphere during the calcination process, so it is difficult to decompose the iron salt into ferric oxide by calcination

Method used

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  • Preparation method of graphene supported ferriferrous oxide nanocomposite
  • Preparation method of graphene supported ferriferrous oxide nanocomposite
  • Preparation method of graphene supported ferriferrous oxide nanocomposite

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Embodiment 1

[0024] 0.05g of graphene and 0.05g of Fe(NO) 3 9H 2 O was added to 40 mL of absolute ethanol, stirred magnetically at a temperature of 60°C for 1 h, weighed 0.004 g of sodium dodecylbenzenesulfonate and added to the above solution, and then continued to stir at room temperature. Weigh 0.0149g of NaOH and dissolve it in 30mL of water. After dissolving, pour it into a separatory funnel and drop it into the above solution at a rate of 15 drops / min. After the titration is completed, continue to stir for 1h. Then it was filtered with a Buchner funnel, and the resulting black powder was washed with deionized water until the pH was 7, and dried in an oven at 60°C for 12 hours. Grind the dried powder, spread the obtained powder in a quartz boat, place the quartz boat in the constant temperature zone of the tube furnace, pass argon gas at a flow rate of 200mL / min for 10min to exhaust the air, and then flow it at 7.5°C / min The heating rate was raised to 450°C under the protection of a...

Embodiment 2

[0026] 0.05g of graphene and 0.05g of FeCl 3 ·6H 2O was added to 60 mL of absolute ethanol, and 0.006 g of sodium dodecylbenzenesulfonate was weighed and added to the above solution, stirred magnetically at a temperature of 60° C. for 1 h, and then continued to stir at room temperature. Weigh 0.0222g of NaOH and dissolve it in 30mL of water. After dissolving, pour it into a separatory funnel and drop it into the above solution at a rate of 15 drops / min. After the titration is completed, continue to stir for 1h. Then it was filtered with a Buchner funnel, and the obtained black powder was washed with deionized water until the pH was 7, and dried in an oven at a temperature of 60°C for 12 hours. Grind the dried powder, spread the obtained powder in a quartz boat, place the quartz boat in the constant temperature zone of the tube furnace, pass argon gas at a flow rate of 200mL / min for 10min to exhaust the air, and then flow it at 7.5°C / min The heating rate was raised to 450°C u...

Embodiment 3

[0028] 0.02g of graphene and 0.01g of Fe(NO) 3 9H 2 O was added to 40 mL of absolute ethanol, stirred magnetically at a temperature of 60°C for 1 h, weighed 0.004 g of sodium dodecylbenzenesulfonate and added to the above solution, and then continued to stir at room temperature. Weigh 0.003g of NaOH and dissolve it in 10mL of water. After dissolving, pour it into a separatory funnel and drop it into the above solution at a rate of 15 drops / min. After the titration is completed, continue to stir for 0.5h. Then it was filtered with a Buchner funnel, and the resulting black powder was washed with deionized water until the pH was 7, and dried in an oven at 80°C for 12 hours. Grind the dried powder, spread the obtained powder in a quartz boat, place the quartz boat in the constant temperature zone of the tube furnace, pass argon gas at a flow rate of 150mL / min for 15min to exhaust the air, and then flow it at 7.5°C / min The heating rate was raised to 450°C under the protection of ...

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Abstract

The invention discloses a preparation method of a graphene supported ferriferrous oxide nanocomposite, comprising the following steps: preparing a precursor by deposition precipitation method, depositing ferric nitrate ninehydrate or ferric chloride hexahydrate on graphene in the form of iron hydroxide by using sodium hydroxide or ammonia to obtain black powder, washing and drying the obtained black powder, grinding the dried black powder, then calcining under the protection of argon, and then cooling, and reducing under the protection of a mixed gas of argon and hydrogen or argon and ammonia gas to obtain the graphene supported ferriferrous oxide nanocomposite. The preparation method is simple and stable. In the obtained composite, ferriferrous oxide is uniformly distributed on graphene and has good interface combination of the substrate graphene, thus the absorbing properties and the like of the composite as a functional material can be improved. The method also can be used for preparing carbon material supported ferriferrous oxide nanocomposites with different substrates by using carbon nanotube, graphite oxide and other carbon materials as the substrate.

Description

technical field [0001] The invention relates to a preparation method of a graphene-supported ferric oxide nanocomposite material, belonging to the technical field of nanocomposite materials. Background technique [0002] Graphene is a new type of two-dimensional carbon nanomaterial obtained by Novoslov of the University of Manchester in 2004 by using adhesive tape to peel off highly oriented graphite. piece". Graphene has excellent physical and chemical properties, and the composite material obtained by using it as a matrix to support oxides has been widely concerned since its discovery. Researchers at home and abroad have also conducted extensive research on the preparation of graphene-loaded ferric oxide composite materials. Due to the good electrical properties of graphene and the magnetic properties of ferric oxide, their composite materials can be used in magnetic resonance Contrast agents, lithium-ion batteries, energy storage and release, and electromagnetic wave ab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K3/00B82Y30/00B82Y40/00
Inventor 李家俊马二龙师春生刘恩佐何春年赵乃勤
Owner TIANJIN UNIV
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