CN109107528A - A kind of preparation method of graphene-supported nickel magnetic composite - Google Patents

A kind of preparation method of graphene-supported nickel magnetic composite Download PDF

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CN109107528A
CN109107528A CN201810967093.3A CN201810967093A CN109107528A CN 109107528 A CN109107528 A CN 109107528A CN 201810967093 A CN201810967093 A CN 201810967093A CN 109107528 A CN109107528 A CN 109107528A
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graphene
solution
graphene oxide
nickel
magnetic composite
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苏孟兴
刘奇
王晶晶
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725th Research Institute of CSIC
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009Magnetic properties
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation

Abstract

A kind of preparation method of graphene-supported nickel magnetic composite, comprising the following steps: choose single layer or few layer graphene oxide water solution, pre-freeze is first carried out to graphene oxide water solution, until graphene oxide solution fully charge;Graphene oxide solution after freezing is subjected to vacuum freeze drying, so that the moisture in solution is distilled by ice is gas;Graphene oxide after vacuum freeze drying is dispersed in ethylene glycol, nickel acetate and hydrazine hydrate are sequentially added, while the molten adjusting PH to 13 of sodium hydroxide is added, then pours into the mixed solution after ultrasound in microwave high pressure reaction kettle, using hydrazine hydrate as reducing agent, keep the temperature under microwave condition;Solution after reaction is washed using suction method, is precipitated, graphene-supported nickel magnetic composite is made after rinsing, drying;Graphene-supported nickel magnetic composite made from the method for the present invention has the characteristic that density is small, coercivity is big, saturation magnetization is high, magnetic product face is big.

Description

A kind of preparation method of graphene-supported nickel magnetic composite
Technical field
The present invention relates to special type function material field, specifically a kind of system of graphene-supported nickel magnetic composite Preparation Method.
Background technique
Electromagnetic shielding material can reflect, absorb, incident electromagnetic wave of decaying, and has electromagnetic wave energy being converted into thermal energy And the function of dissipating or electromagnetic wave is made to disappear by interference, the transmission of electromagnetic wave can be blocked to protect sensitive equipment not by external Electromagnetic Interference, or shielding electromagnetic wave emission source reduce the diffusive transport of its electromagnetic wave.Currently, electromagnetic shielding material all exists The disadvantages of absorption band is narrow, density is big, therefore, the small electromagnetic shielding material of exploitation shielding bandwidth, density become research hotspot. Graphene is a kind of new carbon found recently, have low-density, the carrier mobility of superelevation, conductivity, thermal conductivity, The properties such as intensity, on the one hand, graphene has unique two-dimension plane structure, is to have now been found that a kind of most thin material, thickness is only For 20 a ten thousandths of hair, therefore there is very big specific surface area, theoretical value reaches 2600m2/ g, and than commonly urge Agent carrier has stronger adsorption capacity, can adsorb more catalyst granules, and then make the activity and selection of catalyst Property is greatly enhanced;On the other hand, graphene has highly stable structure and excellent mechanical characteristic, due to graphite C-C key in the planar structure of alkene is connected by covalent bond, and when exposed to external forces, carbon atom face only can be curved under external force Song deformation, adapts to external force without rearranging, to maintain the stability of structure.Recent studies suggest that reduction graphite Its impedance matching property not only can be improved in remaining defect and group in olefinic oxide, can also it be enable to be converted to Fermi rapidly Grade state, can also occur the dielectric relaxor of defect and the electronics dipole relaxation of group, these are conducive to scatter and absorb electromagnetism Wave.
About carbon nanotube loaded inorganic nano-particle, there are many researchs, since graphene is found, increasingly More research begins to focus on the inorganic functional of graphene.Pass through the inorganic nano of graphene and many kinds of different structures and property Particle progress is compound, has prepared the nano hybridization body of miscellaneous novel graphene-inorganic nano-particle, has opened stone Black alkene is more widely applied range.And it is largely used for the modified research work of inorganic functional graphite alkene both at home and abroad at present Electroless plating method is applied to graphene modification and controls surface particle size still belong to a problem by the method for coreduction in situ.Cause This is badly in need of a kind of preparation method of graphene-supported nickel magnetic composite, can improve manufacturing cycle present in existing method Longer, strong acid influences the lower problem of saturation magnetization value of metal nickel content and resulting materials.
Summary of the invention
The purpose of the present invention is to solve the deficiency of above-mentioned technical problem, the present invention proposes a kind of graphene-supported nickel magnetic The preparation method of property composite material passes through hydrothermal process carried magnetic on the surface of graphene using graphene oxide as matrix Nanometer nickel composite material, develops lightweight broad-band electromagnetic shielding material, has preferable electromagnetic performance.
Present invention deficiency to solve above-mentioned technical problem and the technical solution adopted is that:
A kind of preparation method of graphene-supported nickel magnetic composite, comprising the following steps:
(1) single layer or few layer graphene oxide water solution are chosen;
(2) pre-freeze is first carried out to graphene oxide water solution, pre-freezing temperature is -50~-10 DEG C, pre-freeze time > 1h, until oxygen Graphite alkene solution fully charge;
(3) graphene oxide solution after freezing is then put into vacuum oven, vacuumizes carry out vacuum freeze drying, freezed Drying temperature is -45~-25 DEG C, and drying time is 5~20h, so that the moisture in graphene oxide solution is directly distilled by ice and is Gas;
(4) graphene oxide after vacuum freeze drying is dispersed in ethylene glycol, then sequentially adds nickel acetate and water Hydrazine is closed, while sodium hydroxide solution is added, PH is adjusted to 13,5~60min of ultrasound;
(5) graphene oxide, nickel ion mixed solution that ultrasound finishes are poured into microwave high pressure reaction kettle, is also with hydrazine hydrate Former agent keeps the temperature 2~18h under 80~200 DEG C of microwave condition, while being constantly stirred during the reaction;
(6) solution after reaction is washed using suction method, is precipitated, and rinse three respectively with deionized water and ethyl alcohol It is secondary, sediment is then put into vacuum oven, 2~12h is dried in vacuo under the conditions of 60~160 DEG C, can be prepared by graphene Nickel-loaded magnetic composite.
Further, the number of plies of few layer graphene oxide is 2~5 layers.
Further, in the step (4), graphene oxide dosage is 0.1~5mg/mL, the dosage of nickel acetate is 10~ 200mg/mL, the dosage of hydrazine hydrate are 5~20mL.
Further, in the step (5), microwave frequency is 2450 ± 50MHz, and microwave power is 0~500W.
It further, include graphene and nano nickel in the graphene-supported nickel magnetic composite.
Further, mass fraction of the graphene in graphene-supported nickel magnetic composite is 10~50%, Its form is to have the sheet of more fold, and piece diameter is 10~12um.
Further, the nano nickel includes metallic Ni particles and nickel oxide, wherein metallic Ni particles be partial size 20~ Irregular polyhedrons between 200nm, nickel oxide are spherosome of the partial size between 50~100nm.
The beneficial effects of the present invention are:
In raw material selection, first is that selecting single layer or few layer graphene as carrier: the number of plies of graphene influences its performance aobvious It writes, selects single layer or the few carrier of layer graphene oxide (less than 5 layers) as composite absorber, form few layer graphite after reacted Alkene plays the advantage of its superior electron mobility and high-specific surface area, has graphene-supported nano nickel magnetic composite Preferable electric conductivity and effectiveness;Second is that introducing nickel ion in graphene oxide solution: in graphene oxide solution In, nickel ion solution, which is added, is dispersed in nickel ion in graphene oxide colloidal solution, and passes through addition PH regulator wound The reaction environment for producing alkalinity makes nickel ion depend on graphene oxide flocculation;Using hydro-thermal method one-step synthesis nano nickel/graphite Alkene composite material
In preparation method, first is that being handled using vacuum freeze drying graphene oxide solution: graphene oxide is first By cryofixation, then make under conditions of low-temperature high-vacuum moisture therein directly distilled by ice achieve the purpose that it is dry, During drying, graphene oxide by the effect of surface tension, can not keep original chemical composition and physical property, It avoids reuniting to greatest extent and be laminated, so that the homoepitaxial in situ for nano nickle granules provides good carrier;Second is that Under microwave condition, in graphene oxide, nickel ion mixed solution, hydrazine hydrate is added as reducing agent, by microwave reaction one Step synthesis nano nickel/graphene composite material, is had using graphene-supported nickel magnetic composite made from the method for the present invention The characteristic that density is small, coercivity is big, saturation magnetization is high, magnetic product face is big, can be used as electromagnetic shielding filler and electromagnetic shielding is made Coating and electromagnetic shielding composite material can substantially weaken electromagnetic radiation intensity, reduce interference of the electromagnetic wave to sensitive equipment, have Higher economic value, has a extensive future.
Detailed description of the invention
Fig. 1 is graphene-nano nickel SEM photograph;
The hysteresis loop of the graphene-supported nanometer nickel composite material of Fig. 2 different Ni contents.
Specific embodiment
The present invention is further elaborated combined with specific embodiments below.
Specific embodiment:
A kind of preparation method of graphene-supported nickel magnetic composite, comprising the following steps:
(1) single layer or few layer graphene oxide water solution are chosen;The number of plies of graphene its performance is influenced it is significant, select single layer or The few carrier of layer graphene oxide (less than 5 layers) as composite absorber forms few layer graphene, plays its superelevation after reacted The advantage of electron mobility and high-specific surface area, make graphene-supported nano nickel magnetic composite have preferable electric conductivity and Effectiveness;
(2) pre-freeze is first carried out to graphene oxide water solution, pre-freezing temperature is -50~-10 DEG C, pre-freeze time > 1h, until oxygen Graphite alkene solution fully charge;Graphene oxide first passes around cryofixation, then makes it under conditions of low-temperature high-vacuum In moisture directly distilled by ice achieve the purpose that it is dry;
(3) graphene oxide solution after freezing is then put into vacuum oven, vacuumizes carry out vacuum freeze drying, freezed Drying temperature is -45~-25 DEG C, and drying time is 5~20h, and during drying, the moisture in graphene oxide solution is straight Connecing by ice distillation is gas, and graphene oxide by the effect of surface tension, can not keep original chemical composition and physical property, It avoids reuniting to greatest extent and be laminated, so that the homoepitaxial in situ for nano nickle granules provides good carrier;
(4) graphene oxide after vacuum freeze drying is dispersed in ethylene glycol, then sequentially adds nickel acetate and water Hydrazine is closed, while sodium hydroxide solution is added, PH is adjusted to 13,5~60min of ultrasound;
(5) graphene oxide, nickel ion mixed solution that ultrasound finishes are poured into microwave high pressure reaction kettle, is also with hydrazine hydrate Former agent keeps the temperature 2~18h under 80~200 DEG C of microwave condition, while being constantly stirred during the reaction;
(6) solution after reaction is washed using suction method, is precipitated, and rinse three respectively with deionized water and ethyl alcohol It is secondary, sediment is then put into vacuum oven, 2~12h is dried in vacuo under the conditions of 60~160 DEG C, can be prepared by graphene Nickel-loaded magnetic composite.
Further, the number of plies of few layer graphene oxide is 2~5 layers.
Further, in the step (4), graphene oxide dosage is 0.1~5mg/mL, the dosage of nickel acetate is 10~ 200mg/mL, the dosage of hydrazine hydrate are 5~20mL.
Further, in the step (5), microwave frequency is 2450 ± 50MHz, and microwave power is 0~500W.
It further, include graphene and nano nickel in the graphene-supported nickel magnetic composite.
Further, mass fraction of the graphene in graphene-supported nickel magnetic composite is 10~50%, Its form is to have the sheet of more fold, and piece diameter is 10~12um.
Further, the nano nickel includes metallic Ni particles and nickel oxide, wherein metallic Ni particles be partial size 20~ Irregular polyhedrons between 200nm, nickel oxide are spherosome of the partial size between 50~100nm.
Embodiment 1
A kind of preparation method of graphene-supported nickel magnetic composite, comprising the following steps:
(1) aqueous solution of single-layer grapheme oxide is chosen;
(2) pre-freeze is first carried out to graphene oxide water solution, pre-freezing temperature is -50~-10 DEG C, pre-freeze time > 1h, until oxygen Graphite alkene solution fully charge;
(3) graphene oxide solution after freezing is then put into vacuum oven, vacuumizes carry out vacuum freeze drying, freezed Drying temperature is -45~-25 DEG C, and drying time is 5~20h, so that the moisture in graphene oxide solution is directly distilled by ice and is Gas;
(4) graphene oxide after vacuum freeze drying is dispersed in ethylene glycol, then sequentially adds nickel acetate and water Hydrazine is closed, while sodium hydroxide solution is added, PH is adjusted to 13,5~60min of ultrasound;Graphene oxide dosage is 2mg/mL, second The dosage of sour nickel is 10mg/mL, and the dosage of hydrazine hydrate is 5mL;
(5) graphene oxide, nickel ion mixed solution that ultrasound finishes are poured into microwave high pressure reaction kettle, is also with hydrazine hydrate Former agent keeps the temperature 2~18h under 80~200 DEG C of microwave condition, while being constantly stirred during the reaction;Microwave frequency For 2450 ± 50MHz, microwave power is 0~500W;
(6) solution after reaction is washed using suction method, is precipitated, and rinse three respectively with deionized water and ethyl alcohol It is secondary, sediment is then put into vacuum oven, 2~12h is dried in vacuo under the conditions of 60~160 DEG C, can be prepared by graphene Nickel-loaded magnetic composite.
Embodiment 2
A kind of preparation method of graphene-supported nickel magnetic composite, comprising the following steps:
(1) few layer graphene oxide water solution is chosen;
(2) pre-freeze is first carried out to graphene oxide water solution, pre-freezing temperature is -50~-10 DEG C, pre-freeze time > 1h, until oxygen Graphite alkene solution fully charge;
(3) graphene oxide solution after freezing is then put into vacuum oven, vacuumizes carry out vacuum freeze drying, freezed Drying temperature is -45~-25 DEG C, and drying time is 5~20h, so that the moisture in graphene oxide solution is directly distilled by ice and is Gas;
(4) graphene oxide after vacuum freeze drying is dispersed in ethylene glycol, then sequentially adds nickel acetate and water Hydrazine is closed, while sodium hydroxide solution is added, PH is adjusted to 13,5~60min of ultrasound;Graphene oxide dosage is 2mg/mL, second The dosage of sour nickel is 50mg/mL, and the dosage of hydrazine hydrate is 8mL;
(5) graphene oxide, nickel ion mixed solution that ultrasound finishes are poured into microwave high pressure reaction kettle, is also with hydrazine hydrate Former agent keeps the temperature 2~18h under 80~200 DEG C of microwave condition, while being constantly stirred during the reaction;Microwave frequency For 2450 ± 50MHz, microwave power is 0~500W;
(6) solution after reaction is washed using suction method, is precipitated, and rinse three respectively with deionized water and ethyl alcohol It is secondary, sediment is then put into vacuum oven, 2~12h is dried in vacuo under the conditions of 60~160 DEG C, can be prepared by graphene Nickel-loaded magnetic composite.
Embodiment 3
A kind of preparation method of graphene-supported nickel magnetic composite, comprising the following steps:
(1) aqueous solution of single-layer grapheme oxide is chosen;
(2) pre-freeze is first carried out to graphene oxide water solution, pre-freezing temperature is -50~-10 DEG C, pre-freeze time > 1h, until oxygen Graphite alkene solution fully charge;
(3) graphene oxide solution after freezing is then put into vacuum oven, vacuumizes carry out vacuum freeze drying, freezed Drying temperature is -45~-25 DEG C, and drying time is 5~20h, so that the moisture in graphene oxide solution is directly distilled by ice and is Gas;
(4) graphene oxide after vacuum freeze drying is dispersed in ethylene glycol, then sequentially adds nickel acetate and water Hydrazine is closed, while sodium hydroxide solution is added, PH is adjusted to 13,5~60min of ultrasound;Graphene oxide dosage is 2mg/mL, second The dosage of sour nickel is 100mg/mL, and the dosage of hydrazine hydrate is 11mL;
(5) graphene oxide, nickel ion mixed solution that ultrasound finishes are poured into microwave high pressure reaction kettle, is also with hydrazine hydrate Former agent keeps the temperature 2~18h under 80~200 DEG C of microwave condition, while being constantly stirred during the reaction;Microwave frequency For 2450 ± 50MHz, microwave power is 0~500W;
(6) solution after reaction is washed using suction method, is precipitated, and rinse three respectively with deionized water and ethyl alcohol It is secondary, sediment is then put into vacuum oven, 2~12h is dried in vacuo under the conditions of 60~160 DEG C, can be prepared by graphene Nickel-loaded magnetic composite.
Embodiment 4
A kind of preparation method of graphene-supported nickel magnetic composite, comprising the following steps:
(1) few layer graphene oxide water solution is chosen;
(2) pre-freeze is first carried out to graphene oxide water solution, pre-freezing temperature is -50~-10 DEG C, pre-freeze time > 1h, until oxygen Graphite alkene solution fully charge;
(3) graphene oxide solution after freezing is then put into vacuum oven, vacuumizes carry out vacuum freeze drying, freezed Drying temperature is -45~-25 DEG C, and drying time is 5~20h, so that the moisture in graphene oxide solution is directly distilled by ice and is Gas;
(4) graphene oxide after vacuum freeze drying is dispersed in ethylene glycol, then sequentially adds nickel acetate and water Hydrazine is closed, while sodium hydroxide solution is added, PH is adjusted to 13,5~60min of ultrasound;Graphene oxide dosage is 2mg/mL, second The dosage of sour nickel is 150mg/mL, and the dosage of hydrazine hydrate is 15mL;
(5) graphene oxide, nickel ion mixed solution that ultrasound finishes are poured into microwave high pressure reaction kettle, is also with hydrazine hydrate Former agent keeps the temperature 2~18h under 80~200 DEG C of microwave condition, while being constantly stirred during the reaction;Microwave frequency For 2450 ± 50MHz, microwave power is 0~500W;
(6) solution after reaction is washed using suction method, is precipitated, and rinse three respectively with deionized water and ethyl alcohol It is secondary, sediment is then put into vacuum oven, 2~12h is dried in vacuo under the conditions of 60~160 DEG C, can be prepared by graphene Nickel-loaded magnetic composite.
Embodiment 5
A kind of preparation method of graphene-supported nickel magnetic composite, comprising the following steps:
(1) few layer graphene oxide water solution is chosen;
(2) pre-freeze is first carried out to graphene oxide water solution, pre-freezing temperature is -50~-10 DEG C, pre-freeze time > 1h, until oxygen Graphite alkene solution fully charge;
(3) graphene oxide solution after freezing is then put into vacuum oven, vacuumizes carry out vacuum freeze drying, freezed Drying temperature is -45~-25 DEG C, and drying time is 5~20h, so that the moisture in graphene oxide solution is directly distilled by ice and is Gas;
(4) graphene oxide after vacuum freeze drying is dispersed in ethylene glycol, then sequentially adds nickel acetate and water Hydrazine is closed, while sodium hydroxide solution is added, PH is adjusted to 13,5~60min of ultrasound;Graphene oxide dosage is 2mg/mL, second The dosage of sour nickel is 200mg/mL, and the dosage of hydrazine hydrate is 20mL;
(5) graphene oxide, nickel ion mixed solution that ultrasound finishes are poured into microwave high pressure reaction kettle, is also with hydrazine hydrate Former agent keeps the temperature 2~18h under 80~200 DEG C of microwave condition, while being constantly stirred during the reaction;Microwave frequency For 2450 ± 50MHz, microwave power is 0~500W;
(6) solution after reaction is washed using suction method, is precipitated, and rinse three respectively with deionized water and ethyl alcohol It is secondary, sediment is then put into vacuum oven, 2~12h is dried in vacuo under the conditions of 60~160 DEG C, can be prepared by graphene Nickel-loaded magnetic composite.
Graphene-supported nano nickel magnetic composite prepared by the present invention, is mainly made of graphene and nano nickel, such as It is the scanning electron microscope (SEM) photograph of graphene-supported nanometer nickel composite material shown in Fig. 1, wherein graphene is matrix, plays carrier and electricity Loss effect is hindered, the mass fraction in graphene-supported nickel magnetic composite is 10~50%, and form is to have more pleat The sheet of wrinkle, piece diameter are 10~12um;Nano nickle granules mainly play magnetic loss effect, and nano nickel includes metallic Ni particles and oxygen Change nickel, wherein metallic Ni particles are irregular polyhedrons of the partial size between 20~200nm, nickel oxide be partial size 50~ Spherosome between 100nm.
As shown in Fig. 2, the hysteresis loop of the graphene-supported nanometer nickel composite material for different Ni contents, from figure Out, graphene-supported its hysteresis loop of nano nickel composite sample of 10% nickel content is almost in straight line, magnetic field not Induced magnetic field is not also generated when disconnected increasing;Nickel additive amount is respectively 20%, 40% and 50% sample, saturation magnetization difference For 20emu/g, 40emu/g and 50emu/g, coercivity is respectively 25Oe, 179Oe and 183Oe;The sample that nickel additive amount is 30% In its magnetic induction intensity be only 8emu/g, but coercivity be it is maximum in several groups of samples, be 205Oe.
The graphene-supported nickel magnetic composite testing result of table 1
Performance detection is carried out to graphene-supported nickel magnetic composite made from embodiment 1-5, the results are shown in Table 1: compound The partial size of material, less than 0.7, illustrates that composite material is lighter less than 20 μm, density;Oil absorption is less than 19g/100g, illustrates oil absorption It is smaller, it can be used for coating for EMI shielding;The specific saturation magnetization of composite material is greater than 5emu/g, from the foregoing, it will be observed that using this hair Graphene-supported nickel magnetic composite made from bright method is with density is small, coercivity is big, saturation magnetization is high, magnetic product face Big characteristic can be used as electromagnetic shielding filler and electromagnetic screen coating and electromagnetic shielding composite material be made, and can substantially weaken electromagnetism Radiation intensity, reduces interference of the electromagnetic wave to sensitive equipment, and economic value with higher has a extensive future.
The foregoing description of the disclosed embodiments, only for can be realized professional and technical personnel in the field or use this Invention.Various modifications to these embodiments will be readily apparent to those skilled in the art, institute herein The General Principle of definition can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, The present invention will not be limited to the embodiments shown herein, and is to fit to special with principles disclosed herein and novelty The consistent widest scope of point.

Claims (7)

1. a kind of preparation method of graphene-supported nickel magnetic composite, which comprises the following steps:
(1) single layer or few layer graphene oxide water solution are chosen;
(2) pre-freeze is first carried out to graphene oxide water solution, pre-freezing temperature is -50 ~ -10 DEG C, pre-freeze time > 1h, until oxidation Graphene solution fully charge;
(3) graphene oxide solution after freezing is then put into vacuum oven, vacuumizes carry out vacuum freeze drying, freezed Drying temperature is -45 ~ -25 DEG C, and drying time is 5 ~ 20h, and making the moisture in graphene oxide solution is directly gas by ice distillation;
(4) graphene oxide after vacuum freeze drying is dispersed in ethylene glycol, then sequentially adds nickel acetate and water Hydrazine is closed, while sodium hydroxide solution is added, PH is adjusted to 13,5~60min of ultrasound;
(5) graphene oxide, nickel ion mixed solution that ultrasound finishes are poured into microwave high pressure reaction kettle, is also with hydrazine hydrate Former agent keeps the temperature 2 ~ 18 h under 80 ~ 200 DEG C of microwave condition, while being constantly stirred during the reaction;
(6) solution after reaction is washed using suction method, is precipitated, and rinse three respectively with deionized water and ethyl alcohol It is secondary, sediment is then put into vacuum oven, 2 ~ 12h is dried in vacuo under the conditions of 60 ~ 160 DEG C, it is negative to can be prepared by graphene Carry nickel magnetic composite.
2. a kind of preparation method of graphene-supported nickel magnetic composite as described in claim 1, which is characterized in that described The number of plies of few layer graphene oxide is 2 ~ 5 layers.
3. a kind of preparation method of graphene-supported nickel magnetic composite as described in claim 1, which is characterized in that described In step (4), graphene oxide dosage is 0.1~5mg/mL, and the dosage of nickel acetate is 10~200mg/mL, the dosage of hydrazine hydrate For 5~20mL.
4. a kind of preparation method of graphene-supported nickel magnetic composite as described in claim 1, which is characterized in that described In step (5), microwave frequency is 2450 ± 50MHz, and microwave power is 0~500W.
5. a kind of preparation method of graphene-supported nickel magnetic composite as described in claim 1, which is characterized in that described It include graphene and nano nickel in graphene-supported nickel magnetic composite.
6. a kind of preparation method of graphene-supported nickel magnetic composite as claimed in claim 5, which is characterized in that described Mass fraction of the graphene in graphene-supported nickel magnetic composite is 10 ~ 50%, and form is the piece for having more fold Shape, piece diameter are 10 ~ 12um.
7. a kind of preparation method of graphene-supported nickel magnetic composite as claimed in claim 5, which is characterized in that described Nano nickel includes metallic Ni particles and nickel oxide, and wherein metallic Ni particles are irregular multi-panel of the partial size between 20~200nm Body, nickel oxide are spherosome of the partial size between 50~100nm.
CN201810967093.3A 2018-08-23 2018-08-23 A kind of preparation method of graphene-supported nickel magnetic composite Pending CN109107528A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109553094A (en) * 2019-01-03 2019-04-02 深圳天元羲王材料科技有限公司 A kind of grapheme platelet liquid phase ultrasonic dispersing method
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

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102974838A (en) * 2012-11-30 2013-03-20 黑龙江大学 Method for preparing graphene loaded nano nickel composite powder material by hydrothermal method
CN103833008A (en) * 2012-11-20 2014-06-04 中国科学院兰州化学物理研究所 Method for preparing graphene at normal temperature
CN105695788A (en) * 2016-04-08 2016-06-22 上海和伍复合材料有限公司 Graphene strengthening nickel base composite material and preparing method thereof
CN105838913A (en) * 2016-04-08 2016-08-10 上海和伍复合材料有限公司 Graphene/nickel composite material and preparation method thereof
CN108321404A (en) * 2018-03-01 2018-07-24 哈尔滨工业大学 A kind of metal or metal oxide/doping type graphene core-shell catalyst carrier and supported catalyst and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103833008A (en) * 2012-11-20 2014-06-04 中国科学院兰州化学物理研究所 Method for preparing graphene at normal temperature
CN102974838A (en) * 2012-11-30 2013-03-20 黑龙江大学 Method for preparing graphene loaded nano nickel composite powder material by hydrothermal method
CN105695788A (en) * 2016-04-08 2016-06-22 上海和伍复合材料有限公司 Graphene strengthening nickel base composite material and preparing method thereof
CN105838913A (en) * 2016-04-08 2016-08-10 上海和伍复合材料有限公司 Graphene/nickel composite material and preparation method thereof
CN108321404A (en) * 2018-03-01 2018-07-24 哈尔滨工业大学 A kind of metal or metal oxide/doping type graphene core-shell catalyst carrier and supported catalyst and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109553094A (en) * 2019-01-03 2019-04-02 深圳天元羲王材料科技有限公司 A kind of grapheme platelet liquid phase ultrasonic dispersing method
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

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