CN105384146B - Graphene-supported nanometer Fe3o4the preparation method of/ZnO composite - Google Patents
Graphene-supported nanometer Fe3o4the preparation method of/ZnO composite Download PDFInfo
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- CN105384146B CN105384146B CN201510900601.2A CN201510900601A CN105384146B CN 105384146 B CN105384146 B CN 105384146B CN 201510900601 A CN201510900601 A CN 201510900601A CN 105384146 B CN105384146 B CN 105384146B
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000012670 alkaline solution Substances 0.000 claims abstract description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 37
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 13
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 12
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000008246 gaseous mixture Substances 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 abstract 1
- 239000006071 cream Substances 0.000 abstract 1
- 229940044631 ferric chloride hexahydrate Drugs 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract 1
- 238000011017 operating method Methods 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 41
- 239000011787 zinc oxide Substances 0.000 description 20
- 239000011701 zinc Substances 0.000 description 15
- 239000000463 material Substances 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000002242 deionisation method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011358 absorbing material Substances 0.000 description 2
- 239000006249 magnetic particle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
-
- 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)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- G—PHYSICS
- G12—INSTRUMENT DETAILS
- G12B—CONSTRUCTIONAL DETAILS OF INSTRUMENTS, OR COMPARABLE DETAILS OF OTHER APPARATUS, NOT OTHERWISE PROVIDED FOR
- G12B17/00—Screening
- G12B17/02—Screening from electric or magnetic fields, e.g. radio waves
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- 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
Abstract
The present invention relates to a kind of graphene-supported nanometer Fe with electro-magnetic screen function3O4/ ZnO composite and preparation method thereof.First it is that ferric chloride hexahydrate is mixed homogeneously with Zn powder, after precipitation, add alkaline solution and graphene oxide solution, suspension is obtained after stirring, then suspension is placed in constant temp. heating in reactor process, centrifugation, after obtaining the freeze-dried process of cream solid, is placed in tube furnace at H2Thermal reduction is carried out, final prepared graphene-supported nanometer Fe under/Ar mixed atmosphere3O4/ ZnO composite.Graphene-supported nanometer Fe prepared by the present invention3O4/ ZnO composite dispersion is high, good water solubility, and magnetic property and capability of electromagnetic shielding are obviously enhanced, and operating procedure is simple, efficiently, it is easy to accomplish industrialization produces and application.
Description
Technical field
The present invention relates to composite, a kind of graphene-supported nanometer Fe with electro-magnetic screen function3O4/ZnO
The preparation method of composite.
Background technology
At present, electromagnetic pollution has become and pollutes continue noise pollution, water, threaten the fourth-largest of human health after air pollution
Public hazards, for preventing electromagnetic pollution, using electromagnetic shielding material to carry out shielding is one of main prevention method, and high shielding effect
The electromagnetic shielding material of rate, low-density and economy type is then the emphasis of research and development.
Graphene has the structure of uniqueness and excellent physicochemical properties, and intensity height have huge specific surface area and
The characteristics such as density is little, become the focus that research worker gets most of the attention.Graphite is dilute before electromagnetic shielding field has good application
Scape, but its shielding mechanism only comes from dielectric loss, it is impossible to reach the shield effectiveness good to low frequency magnetic field.
In order to make electromagnetic shielding material reach shield effectiveness in broader frequency range, the introducing of magnetic material is must
Indispensable, because of it, there is the magnetic property of skin effect, small-size effect and excellence, development containing ferritic nano-particle
Become the most ripe electromagnetic wave absorbing material, there is the features such as strong, the low cost of absorption；Such as:
CN104163919A discloses the preparation method of a kind of absorbing material, polyaniline/graphene oxide/tetra-oxygen of preparation
Changing three iron composite materials, to have electromagnetic wave absorption strong, absorption band width and the little feature of density.
CN101767767A discloses a kind of ferroso-ferric oxide/zinc oxide core to frequency electromagnetic waves with strong absorption characteristic
The preparation of shell nanometer rod composite material.
Summary of the invention
The present invention is directed to compound dielectric properties and the magnetic property that can be effectively improved material of Graphene and magnetic-particle, have
Effect strengthens the feature of capability of electromagnetic shielding, it is provided that a kind of graphene-supported nanometer Fe3O4The preparation method of/ZnO composite, no
Add any surfactant, obtain the graphene-supported nanometer Fe of high conductivity3O4/ ZnO composite, the addition of magnetic-particle
There is provided magnetic loss for material, make absorbed shield effectiveness be improved, and preparation technology is simple, low cost, it is easy to accomplish produce
Industry metaplasia is produced and application.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of graphene-supported nanometer Fe3O4/ ZnO composite, it is with Graphene as carrier, nanometer Fe3O4/ ZnO is combined
Thing is distributed in graphenic surface, or graphene nanometer sheet is attached to Fe3O4/ ZnO complex surfaces forms package structure.
Above-mentioned graphene-supported nanometer Fe3O4The preparation method of/ZnO composite, comprises the steps:
(1) Zn powder and FeCl that mass ratio is 0.04 ~ 0.12:1 are taken3·6H2O adds in deionized water, at 30 ~ 50 DEG C
Stirring 0.5 more than h under water bath, mixing speed is more than 200r/min, after mix homogeneously, instills alkaline solution, regulation mixing
The pH of liquid is 9 ~ 12, continues stirring, and duration is more than 30min, until mix homogeneously, described Zn powder is graininess or lamellar, mesh
Number is more than 90% more than 400 mesh, Zn content, FeCl3·6H2O solution concentration is 0.01 ~ 2mol/L；
(2) according to FeCl3·6H2O: graphene oxide is that the mass ratio of 1.75 ~ 10.5:1 weighs graphene oxide, is dissolved in
In deionized water, preparing graphene oxide water solution mass concentration is 0.05 ~ 3%, is added in the suspension of step (1), stirs
Mix uniformly, stand-by；
(3) being placed in closed reactor by the mixed solution that step (2) obtains, at a temperature of 160 ~ 200 DEG C, hydro-thermal is anti-
Answer 5 ~ 12 h；
(4) taking out the mixed liquor after step (3) has been reacted and cooled down, through filtering, centrifuging process carries out solid-liquid separation, point
After the freeze-dried process of solid after from, obtain graphene-supported Fe3O4The predecessor of/ZnO composite；
(5) predecessor step (4) obtained is through calcination processing, final prepared graphene-supported Fe3O4/ ZnO composite wood
Material.
Using the present invention of technique scheme, compared with prior art, it provides the benefit that:
1. due to Graphene, there is good electric conductivity, the Fe of load3O4With ZnO nano even particle distribution, and it is combined
Not containing other impurity in material, particle size is controlled, and lower cost for material, and economic cost performance is high, therefore preparation technology letter
Single, it is easy to accomplish industrialization produces and application；
2. due to graphene-supported nanometer Fe3O4/ ZnO composite dispersion is high, good water solubility, magnetic property and electromagnetic screen
Covering performance to be obviously enhanced, the composite electromagnetic shield materials that therefore exploitation has dielectric loss and magnetic loss simultaneously has important
Meaning.
As preferably, the present invention further technical scheme is:
Step (1) neutral and alkali solution is: NaOH solution, KOH solution, ammonia, Ba (OH)2Solution, Na2CO3In solution one
Plant or several.
In step (4), centrifugal separation process uses various centrifuge, reaches solid-liquid separation purpose.
In step (4), lyophilization condition is: freeze temperature maintains-50 ~ 30 DEG C, freeze-drying time 10 ~ 40 h, vacuum
1~300Pa。
In step (5), calcine technology is under argon hydrogen gaseous mixture protective condition, is warmed up to 200 ~ 400 DEG C, is incubated 2 ~ 6 h,
After reaction terminates, dropping to room temperature in gas shield, argon hydrogen gaseous mixture gas ratio is for 95:5.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further elaborated, but embodiment does not constitute any restriction to the present invention.
Embodiment 1:
(1) Zn powder and FeCl that mass ratio is 0.04:1 are taken3·6H2O adds in deionized water, at the water bath of 50 DEG C
Lower stirring 0.5 h, mixing speed 200r/min, after mix homogeneously, instill NaOH solution, the pH of regulation mixed liquor is 9, continues to stir
Mixing, duration is more than 30min, until mix homogeneously；Described Zn powder is graininess or lamellar, and mesh number is more than 400 mesh, and Zn content is big
In 90%, FeCl3·6H2O solution concentration is 0.01mol/L.
(2) according to FeCl3·6H2O: graphene oxide is that the mass ratio of 1.75:1 weighs graphene oxide, is dissolved in deionization
In water, preparing graphene oxide water solution mass concentration is 0.05%, is added in the suspension of step (1), stirs,
Stand-by.
(3) mixed solution that step (2) obtains is placed in closed reactor, hydro-thermal reaction 12 at a temperature of 160 DEG C
h。
(4) taking out the mixed liquor after step (3) has been reacted and cooled down, through filtering, centrifuging process carries out solid-liquid separation, point
After the freeze-dried process of solid after from, obtain graphene-supported Fe3O4The predecessor of/ZnO composite.
(5) by the predecessor that obtains under argon hydrogen gaseous mixture (95:5) protective condition, it is warmed up to 200 DEG C, is incubated 6 h, instead
After should terminating, drop to room temperature in gas shield, final prepared graphene-supported Fe3O4/ ZnO composite.
Embodiment 2:
(1) Zn powder and FeCl that mass ratio is 0.08:1 are taken3·6H2O adds in deionized water, at the water bath of 30 DEG C
Lower stirring 1 h, mixing speed 500r/min, after mix homogeneously, instill KOH solution, the pH of regulation mixed liquor is 12, continues to stir
Mixing, duration is more than 30min, until mix homogeneously；Described Zn powder is graininess or lamellar, and mesh number is more than 400 mesh, and Zn content is big
In 90%, FeCl3·6H2O solution concentration is 0.1mol/L.
(2) according to FeCl3·6H2O: graphene oxide is that the mass ratio of 7:1 weighs graphene oxide, is dissolved in deionized water
In, preparing graphene oxide water solution mass concentration is 3%, is added in the suspension of step (1), stirs, stand-by.
(3) mixed solution that step (2) obtains is placed in closed reactor, hydro-thermal reaction 5 at a temperature of 180 DEG C
h。
(4) taking out the mixed liquor after step (3) has been reacted and cooled down, through filtering, centrifuging process carries out solid-liquid separation, point
After the freeze-dried process of solid after from, obtain graphene-supported Fe3O4The predecessor of/ZnO composite.
(5) by the predecessor that obtains under argon hydrogen gaseous mixture (95:5) protective condition, it is warmed up to 300 DEG C, is incubated 4 h, instead
After should terminating, drop to room temperature in gas shield, final prepared graphene-supported Fe3O4/ ZnO composite.
Embodiment 3:
(1) Zn powder and FeCl that mass ratio is 0.04:1 are taken3·6H2O adds in deionized water, at the water bath of 40 DEG C
Lower stirring 1.5 h, mixing speed 500r/min, after mix homogeneously, instill Na2CO3Solution, the pH of regulation mixed liquor is 10, continues
Stirring, duration is more than 30min, until mix homogeneously；Described Zn powder is graininess or lamellar, and mesh number is more than 400 mesh, Zn content
More than 90%, FeCl3·6H2O solution concentration is 2mol/L.
(2) according to FeCl3·6H2O: graphene oxide is that the mass ratio of 10.5:1 weighs graphene oxide, is dissolved in deionization
In water, preparing graphene oxide water solution mass concentration is 2%, is added in the suspension of step (1), stirs, treat
With.
(3) mixed solution that step (2) obtains is placed in closed reactor, hydro-thermal reaction 12 at a temperature of 200 DEG C
h。
(4) taking out the mixed liquor after step (3) has been reacted and cooled down, through filtering, centrifuging process carries out solid-liquid separation, point
After the freeze-dried process of solid after from, obtain graphene-supported Fe3O4The predecessor of/ZnO composite.
(5) by the predecessor that obtains under argon hydrogen gaseous mixture (95:5) protective condition, it is warmed up to 400 DEG C, is incubated 6 h, instead
After should terminating, drop to room temperature in gas shield, final prepared graphene-supported Fe3O4/ ZnO composite.
Embodiment 4:
(1) Zn powder and FeCl that mass ratio is 0.12:1 are taken3·6H2O adds in deionized water and mixes, the water-bath of 50 DEG C
Stirring 1.5 h, mixing speed 400r/min under environment, after mix homogeneously, instill ammonia, the pH of regulation mixed liquor is 12, continues
Stirring, duration is more than 30min, until mix homogeneously；Described Zn powder is graininess or lamellar, and mesh number is more than 400 mesh, Zn content
More than 90%, FeCl3·6H2O solution concentration is 1.5mol/L.
(2) according to FeCl3·6H2O: graphene oxide is that the mass ratio of 10.5:1 weighs graphene oxide, is dissolved in deionization
In water, preparing graphene oxide water solution mass concentration is 1%, is added in the suspension of step (1), stirs, treat
With.
(3) mixed solution that step (2) obtains is placed in closed reactor, hydro-thermal reaction 5 at a temperature of 200 DEG C
h。
(4) taking out the mixed liquor after step (3) has been reacted and cooled down, through filtering, centrifuging process carries out solid-liquid separation, point
After the freeze-dried process of solid after from, obtain graphene-supported Fe3O4The predecessor of/ZnO composite.
(5) by the predecessor that obtains under argon hydrogen gaseous mixture (95:5) protective condition, it is warmed up to 350 DEG C, is incubated 6 h, instead
After should terminating, drop to room temperature in gas shield, final prepared graphene-supported Fe3O4/ ZnO composite.
The foregoing is only the detailed description of the invention of the present invention, not thereby limit to the interest field of the present invention, all utilizations
The equivalence change that description of the invention content is made, within being both contained in the interest field of the present invention.
Claims (5)
1. a graphene-supported nanometer Fe3O4The preparation method of/ZnO composite, described graphene-supported nanometer Fe3O4/
ZnO composite with Graphene as carrier, nanometer Fe3O4/ ZnO complex is distributed in graphenic surface, or graphene nanometer sheet is attached
At Fe3O4/ ZnO complex surfaces forms package structure；It is characterized in that, comprise the steps:
(1) Zn powder and FeCl that mass ratio is 0.04 ~ 0.12:1 are taken3·6H2O adds in deionized water, the water-bath of 30 ~ 50 DEG C
Stirring 0.5 more than h under environment, mixing speed is more than 200r/min, after mix homogeneously, instills alkaline solution, regulation mixed liquor
PH is 9 ~ 12, continues stirring, and duration is more than 30min, until mix homogeneously, described Zn powder is graininess or lamellar, and mesh number is big
In 400 mesh, Zn content is more than 90%, FeCl3·6H2O solution concentration is 0.01 ~ 2mol/L；
(2) according to FeCl3·6H2O: graphene oxide is that the mass ratio of 1.75 ~ 10.5:1 weighs graphene oxide, be dissolved in from
In sub-water, preparing graphene oxide water solution mass concentration is 0.05 ~ 3%, is added in the suspension of step (1), and stirring is all
Even, stand-by；
(3) mixed solution that step (2) obtains is placed in closed reactor, at a temperature of 160 ~ 200 DEG C hydro-thermal reaction 5 ~
12 h；
(4) taking out the mixed liquor after step (3) has been reacted and cooled down, through filtering, centrifuging process carries out solid-liquid separation, after separation
The freeze-dried process of solid after, obtain graphene-supported Fe3O4The predecessor of/ZnO composite；
(5) predecessor step (4) obtained is through calcination processing, final prepared graphene-supported Fe3O4/ ZnO composite.
Graphene-supported nanometer Fe the most according to claim 13O4The preparation method of/ZnO composite, it is characterised in that:
Step (1) neutral and alkali solution is: NaOH solution, KOH solution, ammonia, Ba (OH)2Solution, Na2CO3One or several in solution
Kind.
Graphene-supported nanometer Fe the most according to claim 13O4The preparation method of/ZnO composite, it is characterised in that:
In step (4), centrifugal separation process uses various centrifuge, reaches solid-liquid separation purpose.
Graphene-supported nanometer Fe the most according to claim 13O4The preparation method of/ZnO composite, it is characterised in that:
In step (4), lyophilization condition is: freeze temperature maintains-50 ~ 30 DEG C, freeze-drying time 10 ~ 40 h, vacuum 1 ~ 300Pa.
Graphene-supported nanometer Fe the most according to claim 13O4The preparation method of/ZnO composite, it is characterised in that:
In step (5), calcine technology is under argon hydrogen gaseous mixture protective condition, is warmed up to 200 ~ 400 DEG C, is incubated 2 ~ 6 h, and reaction terminates
After, dropping to room temperature in gas shield, argon hydrogen gaseous mixture gas is than for 95:5.
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| CN107333460B (en) * | 2017-06-30 | 2019-05-10 | 河北大学 | A kind of preparation method of graphene-based metal composite absorbing material |
| CN108083266B (en) * | 2017-12-29 | 2021-07-20 | 辽宁工程技术大学 | Method for preparing graphene with wave-absorbing property by reducing graphene oxide with zinc powder |
| CN109342613B (en) * | 2018-09-18 | 2021-07-23 | 山东省分析测试中心 | Method for analyzing phenolic endocrine disruptors in beverage |
| CN110964480A (en) * | 2018-09-30 | 2020-04-07 | 山东欧铂新材料有限公司 | Graphene oxide/ferroferric oxide/zinc oxide composite material, preparation method thereof and graphene-based magnetic heat-conducting wave-absorbing material |
| CN110278702B (en) * | 2019-06-04 | 2021-02-19 | 江南石墨烯研究院 | High-stretch high-elasticity electromagnetic shielding composite material and preparation method thereof |
| CN110379636B (en) * | 2019-06-06 | 2021-05-11 | 东南大学 | Preparation of Zn ion doped Fe3O4Method for preparing hollow sphere-graphene electrode material |
| CN114700037A (en) * | 2022-03-25 | 2022-07-05 | 南通三善环保科技有限公司 | Active carbon composite material and process |
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| KR101286106B1 (en) * | 2011-05-30 | 2013-07-16 | 한국과학기술연구원 | The method for producing graphene by chemical exfoliation |
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| Design, Synthesis, and Characterization of Graphene-Nanoparticle Hybrid Materials for Bioapplications.;Perry T. Yin, Shreyas Shah, Manish Chhowalla, and Ki-Bum Lee.;《Chemical Reviews》;20150218;第115卷;第2483-2531页 * |
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