CN106311248A - Zinc ferrite/carbon/zinc oxide nanocomposite material and preparation method thereof - Google Patents
Zinc ferrite/carbon/zinc oxide nanocomposite material and preparation method thereof Download PDFInfo
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- CN106311248A CN106311248A CN201610670201.1A CN201610670201A CN106311248A CN 106311248 A CN106311248 A CN 106311248A CN 201610670201 A CN201610670201 A CN 201610670201A CN 106311248 A CN106311248 A CN 106311248A
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 65
- 229910001308 Zinc ferrite Inorganic materials 0.000 title claims abstract description 56
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000463 material Substances 0.000 title claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910002090 carbon oxide Inorganic materials 0.000 title claims abstract description 21
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 7
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000002131 composite material Substances 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000002105 nanoparticle Substances 0.000 claims abstract description 14
- 239000002077 nanosphere Substances 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000011065 in-situ storage Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 32
- 239000011701 zinc Substances 0.000 claims description 29
- 239000008187 granular material Substances 0.000 claims description 28
- 238000003786 synthesis reaction Methods 0.000 claims description 25
- 230000015572 biosynthetic process Effects 0.000 claims description 23
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 19
- 229910052725 zinc Inorganic materials 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 229910052681 coesite Inorganic materials 0.000 claims description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 229910052682 stishovite Inorganic materials 0.000 claims description 9
- 229910052905 tridymite Inorganic materials 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 229950000845 politef Drugs 0.000 claims description 8
- 238000010276 construction Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 22
- 235000001727 glucose Nutrition 0.000 description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 9
- 239000008103 glucose Substances 0.000 description 9
- 230000005415 magnetization Effects 0.000 description 7
- 238000004627 transmission electron microscopy Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- -1 ZnO compound Chemical class 0.000 description 3
- 210000001742 aqueous humor Anatomy 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005307 ferromagnetism Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000012621 metal-organic framework Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
- 150000002304 glucoses Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- B01J35/39—
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/40—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials of magnetic semiconductor materials, e.g. CdCr2S4
Abstract
The invention discloses a zinc ferrite/carbon/zinc oxide nanocomposite material and a preparation method thereof. The material is a zinc ferrite/carbon/zinc oxide nanocomposite material with a hollow structure, and the chemical formula of the material is ZnFe2O4/C/ZnO; the preparation method of the material comprises the step that by utilizing Fe3O4@C hollow spheres as a template, under the condition of solvent heating, ZnFe2O4/C/ZnO composite hollow nano particles which are uniform in size and regular in morphology are obtained through an in-situ reaction, wherein the size is about 350 nm, and the morphology is of a hollow spherical structure. According to the zinc ferrite/carbon/zinc oxide nanocomposite material and the preparation method thereof, the fact that the ZnFe2O4@C@ZnO composite nano hollow spheres are synthesized by taking the Fe3O4@C hollow nano spheres as the template is proposed for the first time; the technology is advanced, and the prepared product has the excellent property; the preparation technology is simple and easy to operate.
Description
Technical field
The present invention relates to field of nano material preparation, relate to the preparation of oxidate nano hollow ball, particularly one and have concurrently
Magnetic, photocatalysis and the ZnFe of glucose detection performance2O4The preparation of/C/ZnO composite hollow nanosphere.
Background technology
ZnO, as a kind of important wide band gap semiconducter, has been widely used in the field such as gas sensor, photocatalysis.
But, owing to the band gap of ZnO is up to 3.2eV, only have the ultraviolet light of short wavelength that it just can be made to produce light induced electron in sunlight
And hole.But in sunlight, the content of ultraviolet light only accounts for 5%, and most visible ray (50%) but cannot excite ZnO, this
Limit its extensive application.In order to solve this problem, by the ZnO of broad-band gap together with the semiconductors coupling of narrow band gap,
It is a kind of to improve sunlight utilization rate, promote its electronics to separate with hole and improve the effective way of its photocatalysis efficiency.
ZnFe2O4It it is the semi-conducting material of a kind of narrow band gap (1.9eV), it is possible to use most visible ray.Additionally, ZnFe2O4Also have
There are good chemical stability and higher ferromagnetism.But quasiconductor ZnFe2O4Under excited by visible light, its light induced electron and
The recombination rate in hole is very fast, and overall utilization ratio is the highest.If by ZnO and ZnFe2O4Be combined with each other formation heterojunction structure,
The light induced electron that can simultaneously facilitate two kinds of quasiconductors is separated by this structure with hole, thus is greatly improved photocatalysis efficiency.Closely
Nian Lai, document reports some about ZnO/ZnFe2O4The synthetic method of composite, specific as follows:
Holland's " alloy and compound magazine " (Journal of Alloys and Compounds, 2013, the 564th
Volume, page 55 62) report under the conditions of hydro-thermal method, add zinc source and source of iron, one-step synthesis ZnFe2O4/ ZnO composite Nano
Grain.The nano-particle that the method obtains does not has regular shape, and agglomeration is serious.
Switzerland's " Chemical Engineering journal " (Chemical Engineering Journal, 2013, volume 217, the 185th
Page 191) report with ZnFe2O4For template, synthesis has the ZnFe of nucleocapsid structure2O4/ ZnO composite nanometer particle.Due to
ZnFe2O4The pattern of self is irregular and size heterogeneity, and the pattern causing the composite nanometer particle of synthesis is the most irregular.
U.S.'s " physical chemistry magazine " (Journal of Physical Chemistry C, 2010, volume 114, the
Page 17455 17459) report a kind of with carbon ball as template, add the zinc source source of iron that mol ratio is 1:2, in the basic conditions,
Form metal hydroxides, by high annealing, obtain the ZnFe of hollow-core construction2O4/ ZnO nano composite.The method obtains
Particle size relatively big, the specific surface area of material is little, is unfavorable for the carrying out of light-catalyzed reaction.Additionally, remove carbon template at high temperature
Time, easily cause caving in of sky spherical structure.
Germany's " advanced material " (Advanced Materials, 2014, volume 26, page 6,622 6628) report
With metal-organic framework materials (MOFs) as presoma, by annealing process, synthesize ZnFe2O4/ ZnO/C nano composite material.This
Planting method building-up process comparatively laborious, equipment and technical conditions require higher.
The U.S. " ACS application material and interface " (ACS Applied Materials&Interfaces, 2015, the 7th
Volume, the 17811-17818 page) report with ZnO sky ball as template, add source of iron, by high-temperature annealing process, synthesized and had
The ZnFe of double-deck empty spherical structure2O4/ ZnO composite nano materials.In the method, the size of ZnO template is at micron order, causes compound receiving
Rice grain is oversize.Particle size is excessive, reduces its specific surface area, is unfavorable for light-catalyzed reaction.
In sum, currently at synthesis pattern rule, size uniformity, there is the ZnFe of hollow-core construction2O4/ ZnO composite Nano
Still there is challenge on material, we have proposed a kind of low cost, easy synthesis ZnFe in the present invention2O4/ ZnO compound air
The method of heart nanosphere.The ZnFe synthesized by this method2O4/ ZnO composite hollow nanosphere have pattern rule, size equal
One (about 400nm) and good dispersibility.Meanwhile, granule prepared by the method, there is preferable ferromagnetism, the composition of product
Controlled with performance, show good application prospect at the aspect such as photocatalytic degradation of dye and glucose detection.
Summary of the invention
The technical problem to be solved is: provide a kind of new preparation ZnFe2O4/ C/ZnO compound nano-hollow sphere
Method, with the disadvantages mentioned above overcoming prior art to exist.
The present invention solves its technical problem and uses following technical scheme:
Zinc ferrite/carbon/zinc oxide nanometer composite material that the present invention provides, be a kind of there is hollow-core construction zinc ferrite/
Carbon/zinc oxide nanometer composite material, its chemical expression is ZnFe2O4/C/ZnO。
Described zinc ferrite/carbon/zinc oxide nanometer composite material, its a size of 320-370nm, its pattern is hollow ball-shape
Structure.
The preparation method of zinc ferrite/carbon/zinc oxide nanometer composite material that the present invention provides, specifically: utilize Fe3O4@C
Empty ball is template, under conditions of solvent heats, obtains size uniformity, the ZnFe of pattern rule by reaction in-situ2O4/C/ZnO
Composite hollow nanometer, the most a size of 320-370nm, pattern is hollow ball-shape structure.
The preparation method of above-mentioned zinc ferrite/carbon/zinc oxide nanometer composite material that the present invention provides, including following step
Rapid:
A, utilizationMethod synthesis SiO2Granule:
(1) ethanol, deionized water, ammonia 25:2:1 by volume is mixed, quickly stir 30min, make ammonia fully divide
Dissipate in reaction system；
(2) 3mL TEOS is added rapidly in above-mentioned solution, quickly stirs, treat that milky occurs in solution, reduce stirring
Speed, continues stirring 4h, after centrifugal for products therefrom, be washed with deionized repeatedly, be finally scattered in deionized water, be made into
Concentration is the solution for standby of 0.6M；
B, synthetic kernel shell structure SiO2@Fe3O4@C nano granule:
(1) 2～6mL above-mentioned silicon balls are taken, centrifugal, with washing with acetone repeatedly, finally it is scattered in 30mL acetone；
(2) adding in above-mentioned suspension by 0.6g ferrocene, ultrasonic 30min, adding 3mL mass fraction is 30%H2O2, stir
Mixing 30min, being sealed in liner is politef, and shell is in the reaction vessel of steel material, reacts 24～48h in 200 DEG C；
After having reacted, naturally cool to room temperature, centrifugal, washing, obtain the SiO with nucleocapsid structure2@Fe3O4@C nano granule；
C, the Fe of synthesis bivalve layer3O4@C sky ball nano-particle:
By the SiO of gained2@Fe3O4@C nano granule, is scattered in the mixed solution of 10mL deionized water and 5mL ammonia,
Stirring 3min, being enclosed in liner is politef, and shell is in the reaction vessel of steel material, reacts 4 in 140 DEG C～160 DEG C
～8h；Naturally cool to room temperature, be washed with deionized three times, obtain the Fe with double-deck empty spherical structure3O4@C nano granule；
D, synthesis ZnFe2O4/ C@/ZnO composite hollow nanosphere:
Use solvent-thermal method, specifically: by Fe3O4@C nano granule is scattered in the mixed solution of acetone, ethanolamine, super
Sound 30min, adds a certain amount of zinc source, and Fe is (6～1) with the mol ratio in zinc source: (0～1), stirs 10min, and being enclosed in liner is
Politef, shell is in the reaction vessel of steel material, reacts 12～36h in 200 DEG C；Again after Magneto separate and washing,
Obtain ZnFe2O4/ C/ZnO composite hollow nanosphere.
In above-mentioned steps D, described acetone: ethanolamine volume ratio is 1:1.
In above-mentioned steps D, described zinc source uses the one in zinc nitrate, zinc acetate, zinc chloride.
In above-mentioned steps D, described zinc source uses zinc acetate.
In above-mentioned steps D, described Fe is 3:2 with the mol ratio in zinc source.
The present invention compared with prior art has a following major advantage:
Propose first with Fe3O4@C hollow nano-sphere is template, synthesizes this ZnFe2O4@C@ZnO compound nano-hollow sphere.
2. technique is advanced, and the product prepared has excellent properties.
Use Fe3O4@C hollow nano-sphere, as template, prepares composite nanometer particle by reaction in-situ, after reaction terminates
It is not required to remove template, effectively avoids the high-temperature annealing process destruction to hollow-core construction, the composite Nano that this kind of method is prepared
Grain structure is stable, and its composition and performance easy-regulating.This compound nano-hollow sphere have homogeneous size, the structure of rule,
Composition and performance easy-regulating, and good dispersibility.In photocatalytic degradation Organic substance and colorimetric determination glucose are tested
Show the performance of excellence.
3. preparation method technique is simply, easily operate.
Owing to using solvent structure, so simple to operate, low cost, the requirement to equipment is low.
Accompanying drawing explanation
Fig. 1 is ferroferric oxide/carbon (Fe3O4@C) hollow Nano granule and zinc ferrite/carbon/zinc oxide (ZnFe2O4/C/
ZnO) X-ray diffractogram of composite hollow nano-particle, wherein@represents cladding.The standard card of ferroso-ferric oxide is JCPDS
No.19-0629；The standard card of zinc ferrite is JCPDS No.89-1011；The standard card of zinc oxide is JCPDS No.79-
0704。
Fig. 2 isSiO prepared by method2The transmission electron microscopy figure of nano-particle.
Fig. 3 is SiO2@Fe3O4The transmission electron microscopy figure of@C nano granule.
Fig. 4 is Fe3O4The transmission electron microscopy figure of@C sky ball nano-particle.
When Fig. 5 is Fe:Zn=6:1, the transmission electron microscopy figure of the sample of preparation.
When Fig. 6 is Fe:Zn=3:1, the transmission electron microscopy figure of the sample of preparation.
When Fig. 7 is Fe:Zn=3:2, the transmission electron microscopy figure of the sample of preparation.
When Fig. 8 is Fe:Zn=1:1, the transmission electron microscopy figure of the sample of preparation.
When Fig. 9 is Fe:Zn=3:2, the scanning electron microscopy of the sample of preparation.
Figure 10 is the magnetization curve of different sample prepared by Fe/Zn ratio.
Figure 11 is the sample according to embodiment 3 preparation, and the activity figure of catalytic degradation methylene blue is (in figure under visible light
Blue curve, i.e. c curve).In figure as a comparison be without catalyst (black curve in figure, i.e. blank), pure ZnO respectively
(red curve in figure, i.e. a curve), pure ZnFe2O4(green curve in figure, i.e. b curve).
Figure 12 is under fluorescent light, uses the sample of embodiment 3 preparation to detect aqueous humor glucose, dense at different glucoses
Under degree, the uv-visible absorption spectra figure of solution.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, but does not limit the present invention.
Embodiment 1:
The present invention proposes a kind of new synthesis and has the zinc ferrite/carbon/zinc oxide nanometer composite material of hollow-core construction, and it is changed
Expression formula is ZnFe2O4/C/ZnO。
This preparation ZnFe2O4The method of/C/ZnO composite hollow nano-particle, mainly comprises the steps that
1. utilizeMethod synthesis SiO2Granule:
(1) ammonia that dehydrated alcohol, deionized water, mass fraction are 30% is mixed for 25:2:1, quickly by volume
Stirring 30min, makes ammonia be well-dispersed in reaction system；
(2) 3mL TEOS (tetraethyl orthosilicate) is added rapidly in above-mentioned solution, quickly stirs, treat that solution occurs milky white
Color, reduces mixing speed, continues stirring 4h, and products therefrom is quickly centrifugal (8000rpm, 3min), is washed with deionized many
Secondary, finally it is scattered in deionized water, is made into the silicon ball solution for standby that concentration is 0.6M.The SiO of this method synthesis2Nanometer
The size of grain is at about 250nm.
2. synthetic kernel shell structure SiO2@Fe3O4@C nano granule:
(1) 4mL above-mentioned silicon ball solution is taken, centrifugal, with washing with acetone repeatedly, finally it is scattered in 30mL acetone (analytical pure)
In, obtain suspension；
(2), during 0.6g ferrocene adds above-mentioned suspension, ultrasonic 30min, adding 3mL mass fraction is the H of 30%2O2, stir
Mixing 30min, being sealed in liner is politef, and shell is in the reaction vessel of steel material, reacts 24h in 200 DEG C.Reaction
After completing, naturally cool to room temperature, centrifugal, washing, obtain the SiO with nucleocapsid structure2@Fe3O4@C nano granule.
3. synthesis bivalve layer Fe3O4@C sky ball nano-particle:
SiO by above-mentioned gained2@Fe3O4@C nano granule, is scattered in mixed solution (water 10mL, the ammonia of water and ammonia
5mL cumulative volume 15mL) in, stir 3min, being enclosed in liner is politef, and shell is in the reaction vessel of steel material, in
150 DEG C of reaction 6h.Naturally cool to room temperature, be washed with deionized three times, obtain the Fe with double-deck empty spherical structure3O4@C receives
Rice grain.
4. synthesis ZnFe2O4/ C/ZnO composite hollow nano-particle:
By Fe3O4@C nano granule is scattered in the mixed solution (volume ratio is 1:1) of acetone, ethanolamine, ultrasonic 30min,
Add Zn (AC)2As zinc source, being that 6:1 adds zinc source according to the mol ratio of Fe Yu zinc source, stir 10min, it is poly-for being enclosed in liner
Tetrafluoroethene, shell is in the reaction vessel of steel material, reacts 24h in 200 DEG C.Separate, washing.I.e. obtain ZnFe2O4@C@
ZnO composite hollow nanosphere.
Embodiment 2:
On the basis of embodiment 1, only regulating the mol ratio of Fe with zinc source to 3:1, other reaction condition is constant.
Embodiment 3:
On the basis of embodiment 1, only regulating the mol ratio of Fe with zinc source to 3:2, other reaction condition is constant.
Embodiment 4:
On the basis of embodiment 1, only regulating the mol ratio of Fe with zinc source to 1:1, other reaction condition is constant.
Fig. 1 represents template Fe3O4The X ray diffracting spectrum of the composite nanometer particle of@C sky ball nano-particle and final synthesis,
In the drawings, that diamond indicia mark is Fe3O4Diffraction maximum；Circular labelling mark is ZnFe2O4Diffraction maximum, triangle mark
What note marked is the diffraction maximum of ZnO.In figure, the curve of lower section is Fe3O4The diffraction curve of@C, is found by contrast, in figure line
Diffraction maximum position and Fe3O4(Emission in Cubic) standard card JCPDS No.19-0629 is consistent, illustrates that we use in experimentation
Fe3O4It is pure phase, there is no impurity.In figure, the curve of top is ZnFe2O4The diffraction curve of/C/ZnO, finds through contrast, figure
Diffraction maximum position in line and ZnFe2O4(Emission in Cubic) standard card JCPDS No.89-1011 and ZnO (hexagonal phase) standard card
JCPDS No.79-0704 is consistent, does not in addition have the appearance at other miscellaneous peaks, illustrate at end product really by ZnFe2O4
With ZnO two phase composition, and free from admixture exists mutually.
Fig. 2-Fig. 8 represents that the sample in the sample and building-up process that optimal synthetic schemes synthesizes is at transmission electron microscope
The data obtained is characterized under (being called for short TEM).Fig. 2 represents utilizationThe SiO of method synthesis2The TEM of granule characterizes picture, shows
The SiO of synthesis in experiment2Granule has well-regulated pattern, and homogeneous size and good monodispersity, size about exists
About 250nm.Fig. 3 represents SiO2@Fe3O4The TEM of@C nano granule characterizes picture, shows Fe3O4It is coated on completely with C shell
SiO2The surface of granule, additionally, granule still keeps good dispersibility.Fig. 4 represents Fe3O4The TEM table of@C sky ball nano-particle
Levy picture, it can be seen that synthesized granule has sky spherical structure, sample topography rule, size uniformity really from data, divide
Dissipate property good.Fig. 5 is that the TEM of the sample of embodiment 1 gained characterizes picture.Fig. 6 is that the TEM of the sample of embodiment 2 gained characterizes
Picture.Fig. 5, Fig. 6 compare discovery with Fig. 4, and the pattern of sample does not occur significant change, illustrate under both ratios, and
There is no the generation of ZnO.Fig. 7 is that the TEM of the sample of embodiment 3 gained characterizes picture, as can be seen from the figure at Fe3O4@C sky ball
The Surface coating of nano-particle ZnO.Fig. 8 is that the TEM of the sample of specific embodiment 4 gained characterizes picture, can from figure
Going out, the surrounding at granule starts a small amount of ZnO nanorod occur, and Zn is described2+Addition should control within this scope.
Fig. 9 is that the sample prepared by optimal synthesis technique characterizes the data obtained under scanning electron microscope (being called for short SEM).
It can be seen that sample tool is well-regulated spherical, and material is had to adhere on surface；Additionally, by granule damaged in Fig. 9
It can be seen that sample has hollow-core construction really.
Figure 10 represents the magnetization curve figure of the sample in the sample and building-up process that optimal synthetic schemes synthesizes, can from figure
To find out, before and after reaction, the coercivity of sample is zero, illustrates that sample is respectively provided with superparamagnetism.In figure, S1 represents Fe3O4@C is empty
The magnetization curve of ball nano-particle, S2 represents by the magnetization curve of the sample prepared by embodiment 1, and S3 represents by embodiment 2 institute
The magnetization curve of the sample of preparation, S4 represents by the magnetization curve of the sample prepared by embodiment 3, and S5 represents by embodiment 4 institute
The magnetization curve of the sample of preparation.By comparing it is found that work as Fe/Zn mol ratio to increase to 3:1 (from S1-S3), sample from 6:0
The magnetic of product gradually strengthens, and ZnFe is described2O4Content is increasing；When Fe/Zn mol ratio continues to increase (S4-S5), the magnetic of sample
Property gradually weaken, illustrate that the content of ZnO is increasing.
Figure 11 is that the light of the visible wavelength (using filter plate to obtain) sent with 50W xenon lamp irradiates optimal synthesis technique and prepares
ZnFe2O4@C@ZnO sample carries out the activity curve of photocatalytic degradation to methylene blue solution, difference as a comparison in Figure 11
It is without catalyst (the blank curve in Figure 11), pure ZnO (a curve in Figure 11), pure ZnFe2O4(the b curve in Figure 11).Logical
Cross contrast to find, the ZnFe of optimal synthesis technique synthesis2O4The activity of@C@ZnO sample degradation methylene blue higher than pure phase ZnO and
Pure phase ZnFe2O4。
Figure 12 is under fluorescent light, uses the glucose in sample detection aqueous solution prepared by optimal synthesis technique, not
With under concentration of glucose, the uv-visible absorption spectra figure of solution.In figure 12 it can be seen that along with the increasing of concentration of glucose
Adding, the absorbance of solution also becomes larger.Sample synthesized in experiment is described, the detection to aqueous humor glucose has the highest
Activity.
By evaluation result, use the sample of the inventive method synthesis, catalytic degradation organic dyestuff under visible light,
And detection aqueous humor glucose aspect has good activity.In four kinds of embodiments, the performance of the sample that embodiment 3 is prepared
Most preferably.
Claims (8)
1. zinc ferrite/carbon/zinc oxide nanometer composite material, is characterized in that a kind of zinc ferrite/carbon/oxygen with hollow-core construction
Changing zinc nano composite material, its chemical expression is ZnFe2O4/C/ZnO。
Zinc ferrite/carbon/zinc oxide nanometer composite material the most according to claim 1, it is characterised in that described zinc ferrite/
Carbon/zinc oxide nanometer composite material, its size is about 350nm, and its pattern is hollow ball-shape structure.
3. a preparation method for zinc ferrite/carbon/zinc oxide nanometer composite material, is characterized in that utilizing Fe3O4@C sky ball is mould
Plate, under conditions of solvent heats, obtains size uniformity, the ZnFe of pattern rule by reaction in-situ2O4/ C/ZnO composite hollow
Nanometer, wherein size is about 350nm, and pattern is hollow ball-shape structure.
The preparation method of zinc ferrite/carbon/zinc oxide nanometer composite material the most according to claim 3, is characterized in that including
Following steps:
A, utilizationMethod synthesis SiO2Granule:
(1) ethanol, deionized water, ammonia 25:2:1 by volume is mixed, quickly stir 30min, make ammonia be well-dispersed in
In reaction system；
(2) 3mL TEOS is added rapidly in above-mentioned solution, quickly stirs, treat that milky occurs in solution, reduce mixing speed,
Continue stirring 4h, after centrifugal for products therefrom, be washed with deionized repeatedly, be finally scattered in deionized water, be made into concentration
Solution for standby for 0.6M；
B, synthetic kernel shell structure SiO2@Fe3O4@C nano granule:
(1) 2～6mL above-mentioned silicon balls are taken, centrifugal, with washing with acetone repeatedly, finally it is scattered in 30mL acetone；
(2) adding in above-mentioned suspension by 0.6g ferrocene, ultrasonic 30min, adding 3mL mass fraction is 30%H2O2, stirring
30min, being sealed in liner is politef, and shell is in the reaction vessel of steel material, reacts 24～48h in 200 DEG C；Instead
After should completing, naturally cool to room temperature, centrifugal, washing, obtain the SiO with nucleocapsid structure2@Fe3O4@C nano granule；
C, the Fe of synthesis bivalve layer3O4@C sky ball nano-particle:
By the SiO of gained2@Fe3O4@C nano granule, is scattered in the mixed solution of 10mL deionized water and 5mL ammonia, stirring
3min, being enclosed in liner is politef, and shell is in the reaction vessel of steel material, reacts 4～8h in 140 DEG C～160 DEG C；
Naturally cool to room temperature, be washed with deionized three times, obtain the Fe with double-deck empty spherical structure3O4@C nano granule；
D, synthesis ZnFe2O4/ C@/ZnO composite hollow nanosphere:
Use solvent-thermal method, specifically: by Fe3O4@C nano granule is scattered in the mixed solution of acetone, ethanolamine, ultrasonic
30min, adds a certain amount of zinc source, and Fe is (6～1) with the ratio (mol ratio) of the amount of the material in zinc source: (0～1), stirring
10min, being enclosed in liner is politef, and shell is in the reaction vessel of steel material, reacts 12～36h in 200 DEG C；Warp again
After Magneto separate and washing, obtain ZnFe2O4/ C/ZnO composite hollow nanosphere.
The preparation method of zinc ferrite/carbon/zinc oxide nanometer composite material the most according to claim 4, is characterized in that in step
In rapid D, described acetone: ethanolamine volume ratio is 1:1.
The preparation method of zinc ferrite/carbon/zinc oxide nanometer composite material the most according to claim 4, is characterized in that in step
In rapid D, described zinc source uses the one in zinc nitrate, zinc acetate, zinc chloride.
The preparation method of zinc ferrite/carbon/zinc oxide nanometer composite material the most according to claim 4, is characterized in that in step
In rapid D, described zinc source uses zinc acetate.
The preparation method of zinc ferrite/carbon/zinc oxide nanometer composite material the most according to claim 4, is characterized in that in step
In rapid D, described Fe is 3:2 with the mol ratio in zinc source.
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| CN107311234A (en) * | 2017-06-28 | 2017-11-03 | 大连理工大学 | A kind of preparation method of zinc oxide/zinc ferrite nano composite material and application |
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