CN108557899A - A kind of graphene-supported ferroferric oxide wave absorbing material and preparation method thereof - Google Patents
A kind of graphene-supported ferroferric oxide wave absorbing material and preparation method thereof Download PDFInfo
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- CN108557899A CN108557899A CN201810616945.4A CN201810616945A CN108557899A CN 108557899 A CN108557899 A CN 108557899A CN 201810616945 A CN201810616945 A CN 201810616945A CN 108557899 A CN108557899 A CN 108557899A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention belongs to field of nanocomposite materials, a kind of graphene-supported ferroferric oxide wave absorbing material and preparation method thereof is disclosed.The present invention loads ferroso-ferric oxide above using graphene oxide as raw material with coprecipitation, then is reduced to graphene/ferroso-ferric oxide.Avoid the high temperature and pressure operation in solvent-thermal method, simple and safe operation；Ferroso-ferric oxide and graphene oxide are tightly combined simultaneously, are not readily separated.The reducing agent that the present invention selects is ascorbic acid, not only it is avoided that the use of high poison reducing agent hydrazine hydrate in conventional method, can also graphene oxide be effectively reduced to graphene, and increase dispersibility of the product in various organic solvents, contribute to its dispersion in the base.
Description
Technical field
The invention belongs to field of nanocomposite materials, more particularly to a kind of graphene-supported ferroferric oxide wave absorbing material and
Preparation method.
Background technology
With popularizing for various electronic products, electromagnetic wave also becomes a kind of new environmental pollution.Electromagnetic wave not only can be right
The work of precision electronic element interferes, and the long-term exposure under electromagnetic wave can also generate health certain influence.And
In military field, aircraft can also be such that our unit is exposed in the monitoring in place the reflection of electromagnetic wave.Therefore, electricity is administered
Magnetic wave pollutes, and a kind of material of energy efficient absorption electromagenetic wave radiation of searching is current one big project.
Traditional absorbing material has ferromagnetic material and metal fine powder etc..However the small and unsuitable height of the electrical conductance of ferromagnetic material
The shielding of frequency electromagnetic waves；And metal fine powder density is big, perishable, not easy to be processed, limitation is larger.
With the development of nanotechnology, people are gradually found that some nano materials with excellent properties.Graphene,
It is monolayer graphite, is a kind of quasi- two-dimensional material of only monolayer thickness.Since it has very good intensity, soft
Toughness, conduction, heat conduction, optical characteristics all obtain in fields such as physics, materialogy, electronic information, computer, aerospaces
Significant progress.Meanwhile the inorganic nano-particle loaded using graphene as matrix is also got the attention.Such as four oxygen
Change three-iron, since graphene has electrical effect, and there is ferroso-ferric oxide magnetic effect, the synergistic effect that the two is combined generation to make
It has wide foreground in electro-magnetic wave absorption field.
The method for preparing graphene-supported ferroso-ferric oxide at present has following two：
(1) solvent-thermal method：The compounds such as ferroso-ferric oxide and graphene and the sodium acetate to work in the reaction are existed
Stirring and dissolving in reducing agent, mixed solution is put into reaction kettle, the method reacted at high temperature.This method is molten
The hot method of agent prepares a kind of method derived on the basis of the method for ferroso-ferric oxide, and this method is simple for process, but is related to height
Warm operation with high pressure has certain security risk；And parameter needed to be considered is excessive in reacting, as temperature, reaction time, reducing agent add
Dispensing ratio of amount and raw material added etc. is difficult to control；Finally obtained product magnetism is weaker, is not easy to be used as absorbing material.
(2) coprecipitation：I.e. in a nitrogen atmosphere, by divalent iron salt, trivalent iron salt and graphene oxide in certain temperature
Lower mixing titrates synthesis ferroso-ferric oxide by sodium hydroxide (or other aqueous slkalis), finally uses hydrazine hydrate or hydroboration
The method of the reducing agents such as sodium reduction.This method is mainly primary raw material by being tied in alkaline solution using ferrous iron and ferric iron
The method that conjunction prepares ferroso-ferric oxide derives to obtain, and the ferriferrous oxide particles that this method obtains are smaller, and preparation condition readily satisfies.
But the use of the reducing agents such as hydrazine hydrate and sodium borohydride has certain risk, has safety hidden in extensive preparation production
Suffer from.Meanwhile dispersion stabilization is poor in organic solvent for obtained graphene/ferroferric oxide compound, is difficult in the base
It is evenly distributed, electro-magnetic wave absorption effect cannot be played well.
In this regard, finding a kind of efficient, the safe method that can be loaded to ferroso-ferric oxide on graphene and what is obtained answer
The dispersion stabilization of condensation material is still current a great problem and research hotspot well.
Invention content
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that offer is a kind of to use Vitamin C
Acid carrys out the safe and efficient method that synthesizing graphite alkene loads ferroferric oxide wave absorbing material as reducing agent.
Another object of the present invention is to provide the graphene-supported ferroferric oxide wave absorbing material of above method preparation.
The purpose of the present invention is realized by following proposal：
A method of with ascorbic acid ferroferric oxide wave absorbing material, master are loaded come synthesizing graphite alkene as reducing agent
Include the following steps：
(1) graphene oxide is dispersed in water to obtain graphene oxide dispersion under ultrasonic wave added；
(2) under nitrogen atmosphere, ferric chloride hexahydrate solution and four chloride hydrates are added into the dispersion liquid in step (1)
The pH of system is adjusted to 9~11, reaction by ferrous iron solution after stirring evenly；
(3) it waits in step (2) after reaction, ascorbic acid being added thereto, the reaction was continued；
(4) after reaction, gained reaction product will be cooled to room temperature in step (3), then uses magnet isolated
Black precipitate after being respectively washed several times with distilled water and ethyl alcohol, is dried in vacuo up to reaction product.
The number of plies of graphene oxide described in step (1) is 1-10 layers, and size is 0.5-50 μm；
A concentration of 0.5~5mgmL of graphene oxide dispersion described in step (1)-1；
Ultrasound described in step (1) refers to 10~30min of supersound process under 50~100W power；
Ferric chloride hexahydrate solution described in step (2) is preferably a concentration of 0.025~0.125gmL-1It is water-soluble
Liquid；The Iron dichloride tetrahydrate solution is preferably a concentration of 0.02~0.125gmL-1Aqueous solution；
The addition of ferric chloride hexahydrate solution and Iron dichloride tetrahydrate solution described in step (2) is preferably with 0.2
The speed of~1 drop/s is added dropwise.
The dosage of dispersion liquid, ferric chloride hexahydrate solution and Iron dichloride tetrahydrate solution described in step (2) meets
The mass ratio of graphene oxide, ferric chloride hexahydrate and Iron dichloride tetrahydrate is 1：1.25~6.25：0.5~6.25；
Adjusting pH value described in step (2) refers to adjusting body at least one of ammonium hydroxide, sodium hydroxide, sodium carbonate
The pH of system；
Reaction described in step (2) refers to 10~60min of reaction at 30~80 DEG C；
The dosage of ascorbic acid described in step (3) meets the graphene oxide in system per 1g and corresponds to 5~10g of addition
Ascorbic acid；
Reaction described in step (3) refer at 30~80 DEG C reaction 1~for 24 hours；
Cleaning described in step (4) is preferably cleaned 3~6 times several times；Drying described in step (4) is preferably 60
DEG C vacuum drying chamber in dry 8h；
A kind of graphene-supported ferroferric oxide wave absorbing material being prepared by the above method.
The present invention compared with the existing technology, has the following advantages and advantageous effect：
The present invention provides a kind of preparation methods of graphene/ferriferrous oxide nano composite material.The method with it is previous
Preparation method compare, advantage is to load ferroso-ferric oxide above with coprecipitation using graphene oxide as raw material, then will
It is reduced to graphene/ferroso-ferric oxide.Avoid the high temperature and pressure operation in solvent-thermal method, simple and safe operation；While four
Being tightly combined for Fe 3 O and graphene oxide, is not readily separated.The reducing agent that the present invention selects is ascorbic acid, can not only be kept away
Exempt from the use of high poison reducing agent hydrazine hydrate in conventional method, moreover it is possible to graphene oxide is effectively reduced to graphene, and increase production
Dispersibility of the object in various organic solvents contributes to its dispersion in the base.
Description of the drawings
Fig. 1 is the XRD diagram of product in embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of the product in embodiment 3；
Fig. 3 is the dispersion performance design sketch of embodiment 1 and the product in comparative example 1.
Fig. 4 is product in embodiment 2 and paraffin with mass ratio 1：1 is uniformly mixed manufactured coaxial style under different-thickness
Electromagnetic wave reflection loss figure.
Specific implementation mode
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Graphene oxide used is provided by Suzhou Tan Feng graphenes Co., Ltd in embodiment, and the number of plies is 1-10 layers, size
It is 0.5-50 μm.Other reagents can routinely be bought unless otherwise specified from market.
Embodiment 1
(1) distilled water of 200mL is added in the four-hole boiling flask for taking a 500mL, and 200mg graphene oxides are then added, close
The dispersion 30min under ultrasonic wave added that is honored as a queen obtains 1mgmL-1Graphene oxide dispersion.At 80 DEG C, under nitrogen atmosphere,
0.025gmL is added dropwise with the rate of two seconds one drops dropwise into flask-1Ferric chloride hexahydrate 10mL and 0.02gmL-1's
Iron dichloride tetrahydrate 5mL after stirring 10min, is added dropwise ammonium hydroxide to the pH=10 of system, reacts 30min inward.
(2) temperature is set as 50 DEG C, 2g ascorbic acid is added into flask, react 6h.After reaction, it is cooled to room
Temperature is detached with magnet, obtains black precipitate, after being respectively washed 3 times with distilled water and ethyl alcohol, is dried in vacuo at 60 DEG C
8h obtains graphene/ferriferrous oxide nano composite material.
The XRD spectra of 1 product of embodiment is as shown in Fig. 1, from figure 1 it appears that the feature diffraction of ferroso-ferric oxide
Peak (220), (311), (400), (422), (511), (440), (533) are corresponding with the crystal form of pure ferroso-ferric oxide.Illustrate stone
The combination of black alkene does not have an impact the crystal habit of ferroso-ferric oxide.
Embodiment 2
(1) distilled water of 200mL is added in the four-hole boiling flask for taking a 500mL, and 200mg graphene oxides are then added, close
The dispersion 30min under ultrasonic wave added that is honored as a queen obtains 1mgmL-1Graphene oxide dispersion.It is past under nitrogen atmosphere at 50 DEG C
0.05gmL is added dropwise with the rate of two seconds one drops dropwise in flask-1Ferric chloride hexahydrate 10mL and 0.04gmL-1Four water
Frerrous chloride 5mL is closed, after stirring 10min, sodium hydroxide solution is added dropwise inward to the pH=11 of system, reacts 10min.
(2) temperature is set as 30 DEG C, 2g ascorbic acid is added into flask, reaction is for 24 hours.After reaction, it is cooled to
Room temperature is detached with magnet, obtains black precipitate, after being respectively washed several times with distilled water and ethyl alcohol, the vacuum at 60 DEG C
Dry 8h obtains graphene/ferriferrous oxide nano composite material.
Embodiment 3
(1) distilled water of 200mL is added in the four-hole boiling flask for taking a 500mL, and 200mg graphene oxides are then added, close
The dispersion 30min under ultrasonic wave added that is honored as a queen obtains 1mgmL-1Graphene oxide dispersion.At 30 DEG C, into flask with two
0.125gmL is added dropwise in the second rate of one drop dropwise-1Ferric chloride hexahydrate 10mL and 0.125gmL-1Four chloride hydrates it is sub-
Iron 10mL after stirring 10min, is added dropwise sodium carbonate liquor to the pH=9 of system, reacts 1h inward.
(2) temperature is set as 80 DEG C, 1g ascorbic acid is added into flask, react 1h.After reaction, it is cooled to room
Temperature is detached with magnet, obtains black precipitate, and after being respectively washed several times with distilled water and ethyl alcohol, vacuum is dry at 60 DEG C
Dry 8h obtains graphene/ferriferrous oxide nano composite material.
The scanning electron microscope (SEM) photograph of 3 product of embodiment is as shown in Fig. 2, as can be seen from Figure 2 ferriferrous oxide nano-particle
It is attached on the surface of graphene.
Comparative example 1：
The ascorbic acid in step (2) is replaced with to the hydrazine hydrate of equivalent with differing only in for embodiment 1.
The product obtained in 2g embodiments 1 and comparative example 1 is taken to be added separately in 10mL acetone solns, ultrasound
It is stood after 10min and observes its dispersion performance, the dispersion performance design sketch of the product obtained in embodiment 1 and comparative example 1 is such as
Shown in Fig. 3, (a), (b), (c) in Fig. 3 and (d) respectively represent stand 1h, 3h, 12h, for 24 hours after photo, wherein left side is
Product in embodiment 1, right side is product in comparative example 1, the product that as can be seen from Figure 3 example 1 obtains
Also possess good dispersibility after standing 12h in acetone, and with the sample that hydrazine hydrate reduction obtains in comparative example 1 in 3h
Just occur apparent sedimentation afterwards, illustrates that the product prepared by present invention ascorbic acid has excellent dispersion stabilization.It is this
Good dispersibility has benefited from the surface that ascorbic acid will also be attached to graphene while redox graphene, to anti-
The only reunion between graphene.
Graphene/ferroso-ferric oxide is a kind of wave absorbing agent, and itself is pulverulence, is wanted and polymeric matrix so general
It is combined into wave-absorber competence exertion its wave-absorbing effect.And this mixed process at present generally be solution mixing method, be exactly
It is uniformly mixed with organic solvent dissolving and is then dried.So stably dispersing row in organic solvent contributes to it in polymer
It is finely dispersed in matrix.And the suction wave principle of graphene be it have high conductivity, form conductive path in the base, from
And pass through electrical loss electromagnetic wave absorption.If it cannot be uniformly dispersed in the base, conductive path cannot be formed, its suction
Wave performance can also decline, therefore good dispersion stabilization is beneficial to graphene/ferroso-ferric oxide poly- in organic solvent
Being uniformly dispersed in object matrix is closed, this is most important for the performance of preparation and its suction wave effect of polymer matrix wave-absorber
's.
By the product obtained in embodiment 2 and paraffin with mass ratio 1：1 is uniformly mixed, and coaxial style is made, with vector net
Network analyzer tests its absorbing property.The results are shown in Figure 4, the as can be seen from Figure 4 material it is maximum inhale intensity of wave be-
28dB, the suction intensity of wave between 8Hz to 15Hz are both greater than -20dB.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (7)
1. a kind of method loading ferroferric oxide wave absorbing material as reducing agent come synthesizing graphite alkene with ascorbic acid, feature
It is to include the following steps：
(1) graphene oxide is dispersed in water to obtain graphene oxide dispersion under ultrasonic wave added；
(2) under nitrogen atmosphere, ferric chloride hexahydrate solution and Iron dichloride tetrahydrate are added into the dispersion liquid in step (1)
The pH of system is adjusted to 9~11, reaction by solution after stirring evenly；
(3) it waits in step (2) after reaction, ascorbic acid being added thereto, the reaction was continued；
(4) after reaction, gained reaction product will be cooled to room temperature in step (3), then uses the isolated black of magnet
Sediment after being respectively washed several times with distilled water and ethyl alcohol, is dried in vacuo up to reaction product.
2. according to claim 1 inhale wave material as reducing agent with ascorbic acid come synthesizing graphite alkene load ferroso-ferric oxide
The method of material, it is characterised in that：
The number of plies of graphene oxide described in step (1) is 1-10 layers, and size is 0.5-50 μm；
A concentration of 0.5~5mgmL of graphene oxide dispersion described in step (1)-1；
Ultrasound described in step (1) refers to 10~30min of supersound process under 50~100W power.
3. according to claim 1 inhale wave material as reducing agent with ascorbic acid come synthesizing graphite alkene load ferroso-ferric oxide
The method of material, it is characterised in that：
Ferric chloride hexahydrate solution described in step (2) is a concentration of 0.025~0.125gmL-1Aqueous solution；Described
Iron dichloride tetrahydrate solution is a concentration of 0.02~0.125gmL-1Aqueous solution；
The dosage of dispersion liquid, ferric chloride hexahydrate solution and Iron dichloride tetrahydrate solution described in step (2) meets oxidation
The mass ratio of graphene, ferric chloride hexahydrate and Iron dichloride tetrahydrate is 1：1.25~6.25：0.5~6.25.
4. according to claim 1 inhale wave material as reducing agent with ascorbic acid come synthesizing graphite alkene load ferroso-ferric oxide
The method of material, it is characterised in that：
Adjusting pH value described in step (2) refers to at least one of ammonium hydroxide, sodium hydroxide, sodium carbonate come regulation system
pH；
Reaction described in step (2) refers to 10~60min of reaction at 30~80 DEG C.
5. according to claim 1 inhale wave material as reducing agent with ascorbic acid come synthesizing graphite alkene load ferroso-ferric oxide
The method of material, it is characterised in that：
The dosage of ascorbic acid described in step (3) meets the graphene oxide in system per 1g and corresponds to the anti-of 5~10g of addition
Bad hematic acid；
Reaction described in step (3) refer at 30~80 DEG C reaction 1~for 24 hours.
6. according to claim 1 inhale wave material as reducing agent with ascorbic acid come synthesizing graphite alkene load ferroso-ferric oxide
The method of material, it is characterised in that：
Cleaning described in step (4) is cleaning 3~6 times several times；Drying described in step (4) is the vacuum drying at 60 DEG C
Dry 8h in case.
7. a kind of graphene-supported ferroso-ferric oxide being prepared according to claim 1~6 any one of them method inhales wave
Material.
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| CN109729707A (en) * | 2019-03-15 | 2019-05-07 | 韩振 | A method of preparing carbon nano tube electromagnetic shielding film |
| CN110256732A (en) * | 2019-04-27 | 2019-09-20 | 华南理工大学 | A kind of ferroso-ferric oxide-graphene-cellulose conduction composite aerogel and preparation method thereof applied to electromagnetic shielding field |
| CN111233046A (en) * | 2020-03-05 | 2020-06-05 | 江苏信息职业技术学院 | Hollow magnetic Fe for magnetorheological fluid3O4Nano-doped microsphere and preparation method thereof |
| CN111943274A (en) * | 2020-08-20 | 2020-11-17 | 清华大学 | Preparation method of green electromagnetic shielding building material |
| CN112848586A (en) * | 2020-12-30 | 2021-05-28 | 中国科学院长春应用化学研究所 | Multilayer electromagnetic shielding composite material based on isolation structure and preparation method and application thereof |
| CN113395888A (en) * | 2021-04-26 | 2021-09-14 | 中国人民解放军96901部队25分队 | Hollow ferroferric oxide/reduced graphene oxide nano composite wave-absorbing material and preparation method thereof |
| CN114703657A (en) * | 2022-04-20 | 2022-07-05 | 浙江理工大学 | Preparation method of coated cotton fabric with efficient electromagnetic wave absorption performance |
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| CN109729707A (en) * | 2019-03-15 | 2019-05-07 | 韩振 | A method of preparing carbon nano tube electromagnetic shielding film |
| CN110256732A (en) * | 2019-04-27 | 2019-09-20 | 华南理工大学 | A kind of ferroso-ferric oxide-graphene-cellulose conduction composite aerogel and preparation method thereof applied to electromagnetic shielding field |
| CN110256732B (en) * | 2019-04-27 | 2021-07-20 | 华南理工大学 | Ferroferric oxide-graphene-cellulose conductive composite aerogel applied to field of electromagnetic shielding and preparation method thereof |
| CN111233046A (en) * | 2020-03-05 | 2020-06-05 | 江苏信息职业技术学院 | Hollow magnetic Fe for magnetorheological fluid3O4Nano-doped microsphere and preparation method thereof |
| CN111943274A (en) * | 2020-08-20 | 2020-11-17 | 清华大学 | Preparation method of green electromagnetic shielding building material |
| CN112848586A (en) * | 2020-12-30 | 2021-05-28 | 中国科学院长春应用化学研究所 | Multilayer electromagnetic shielding composite material based on isolation structure and preparation method and application thereof |
| CN113395888A (en) * | 2021-04-26 | 2021-09-14 | 中国人民解放军96901部队25分队 | Hollow ferroferric oxide/reduced graphene oxide nano composite wave-absorbing material and preparation method thereof |
| CN114703657A (en) * | 2022-04-20 | 2022-07-05 | 浙江理工大学 | Preparation method of coated cotton fabric with efficient electromagnetic wave absorption performance |
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