CN105540681A - Cage-shaped ferric oxide hollow ball and preparation method thereof - Google Patents
Cage-shaped ferric oxide hollow ball and preparation method thereof Download PDFInfo
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- CN105540681A CN105540681A CN201610028536.3A CN201610028536A CN105540681A CN 105540681 A CN105540681 A CN 105540681A CN 201610028536 A CN201610028536 A CN 201610028536A CN 105540681 A CN105540681 A CN 105540681A
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- Prior art keywords
- ferric oxide
- hollow ball
- oxide hollow
- preparation
- caged
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 32
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 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 claims abstract description 18
- 239000008103 glucose Substances 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 229910001448 ferrous ion Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 229940010514 ammonium ferrous sulfate Drugs 0.000 abstract 3
- 238000001035 drying Methods 0.000 abstract 2
- 239000011259 mixed solution Substances 0.000 abstract 2
- 239000000243 solution Substances 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- -1 ferrous iron ions Chemical class 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- 239000000463 material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 3
- 239000013543 active substance Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- 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
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention belongs to the technical field of inorganic semiconductor composites, and particularly relates to a cage-shaped ferric oxide hollow ball and a preparation method thereof. The preparation method of the cage-shaped ferric oxide hollow ball comprises the following steps: (1) dissolving ammonium ferrous sulfate in deionized water, and performing ultrasonic treatment until the ammonium ferrous sulfate is completely dissolved; (2) dissolving glucose in the deionized water; (3) uniformly mixing an ammonium ferrous sulfate solution obtained in the step (1) with a glucose solution obtained in the step (2) so as to obtain a mixed solution, transferring the mixed solution into a reaction kettle, and placing the reaction kettle into a drying oven for heating for 22-26 hours at 160-200 DEG C, wherein the molar ratio of glucose to ferrous iron ions is (5-15):1; (4) cooling samples obtained in the step (3), washing the cooled samples, and drying the washed samples to be kept for a night; (5) calcinating the samples obtained in the step (4) for 5-6 hours at 530-570 DEG C so as to obtain the cage-shaped ferric oxide hollow spheres. The method provided by the invention is simple, mild, green, pollution-free, and good in repeatability, and besides, no surfactant is used in the course of the method.
Description
Technical field
The invention belongs to inorganic semiconductor technical field of composite materials, be specifically related to a kind of caged ferric oxide hollow ball and preparation method thereof.
Background technology
Fe
2o
3belong to hexagonal system, its lattice parameter is respectively a=0.5043nm, b=1.375nm.Fe
2o
3be a kind of semiconductor material, its energy gap is 2.1eV, has very strong absorption in visible region, makes it in photochemical catalysis, photochromic, gas sensor, have good using value.Nanometer Fe
2o
3it is the very important metal oxide of a class of nanometer novel material, its chemical property is more stable, catalytic activity is high, has all fundamental characteristics of nano material, is usually used in coating, catalyzer, magneticsubstance, rubber, papermaking, pottery, glass, medicine and other fields.Therefore, character and the application of studying the iron oxide material of Nano grade have very important practical significance.
The structure of material determines himself performance to a great extent, comprises the pattern of material, crystallinity, size etc., and these aspects are closely bound up with the synthetic method adopted and preparation process.Hydrothermal method is a kind of method utilizing the mechanism of dissolution-recrystallization to prepare specific product, is particularly widely used in preparation nano material, the method products therefrom has that particle purity is high, good dispersity and the advantage such as crystal formation is good.
Summary of the invention
The object of the present invention is to provide a kind of caged ferric oxide hollow ball and preparation method thereof.Described preparation method is simply gentle, and green non-pollution is reproducible, and inapplicable any tensio-active agent in process.
The present invention adopts following technical scheme:
A preparation method for caged ferric oxide hollow ball, it comprises the following steps:
(1) ferrous ammonium sulphate is dissolved in deionized water, ultrasonic to dissolving completely;
(2) glucose is dissolved in deionized water;
(3) by the l ferrous ammonium sulfate solution of step (1) gained with mix in the glucose solution of step (2) gained after transfer in reactor, and be placed in baking oven and heat 22 ~ 26 hours at 160 ~ 200 DEG C, wherein the mol ratio of glucose and ferrous ion is 5-15:1;
(4) sample of step (3) gained cooled, wash, dry and spend the night;
(5) sample of step (4) gained is calcined 5 ~ 6 hours at 530 ~ 570 DEG C, obtain caged ferric oxide hollow ball.
The volumetric molar concentration of described l ferrous ammonium sulfate solution is 0.2 ~ 0.5mol/L.
The volumetric molar concentration of described glucose solution is 1.0 ~ 4.0mol/L.
First use deionized water wash three times in described step (4), then use washing with alcohol three times.
In described step (4), bake out temperature is 70 ~ 90 DEG C.
The caged ferric oxide hollow ball adopting described method to prepare, size uniform, diameter is between 670 ~ 1500nm, and the shell thickness of ferric oxide is between 60 ~ 180nm.
The present invention adopts hydrothermal method, take glucose as carbon ball starting material, take ferrous ammonium sulphate as source of iron, then removes the ferric oxide hollow ball of obtained caged after carbonaceous core through calcining.Described preparation method is simply gentle, and green non-pollution is reproducible, and inapplicable any tensio-active agent in process.
Accompanying drawing explanation
The SEM figure of the caged ferric oxide hollow ball of Fig. 1 prepared by embodiment 1.
The SEM figure of the caged ferric oxide hollow ball of Fig. 2 prepared by embodiment 2.
The SEM figure of the caged ferric oxide hollow ball of Fig. 3 prepared by embodiment 3.
The XRD figure of the caged ferric oxide hollow ball of Fig. 4 prepared by embodiment 1.
Embodiment
The present invention is further described below by way of embodiment, as known by the technical knowledge, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.
Embodiment 1
5.88g ferrous ammonium sulphate is dissolved in 40mL deionized water, ultrasonic to dissolving completely.13.5g glucose is dissolved in 27mL deionized water, is stirred to dissolving, copperas solution solution is mixed with glucose solution, proceed to 100mL reactor, at being placed in 180 DEG C, baking oven, heat 24h.After heating, be cooled to room temperature, the sample of gained is washed, first use deionized water wash three times, then use washing with alcohol three times, then dry at 80 DEG C and spend the night.The sample of gained is calcined 5 ~ 6 hours at 550 DEG C, obtains caged ferric oxide hollow ball, to the present embodiment product (Fe
2o
3hollow ball) carry out scanning electron microscope to observe its microscopic appearance, result as shown in Figure 1, prepared Fe
2o
3sample is size uniform, and diameter is in the hollow ball shape structure of about 670 ~ 700nm, and the shell of ferric oxide is by 1 ~ 3 Fe
2o
3small-particle forms, and thickness is between 60 ~ 180nm.To the present embodiment product (Fe
2o
3hollow ball) carry out X-ray powder diffraction analysis, as shown in Figure 4, there is Fe in result
2o
3characteristic peak, and consistent with standard card.
Embodiment 2
5.88g ferrous ammonium sulphate is dissolved in 40mL deionized water, ultrasonic to dissolving completely.27g glucose is dissolved in 54mL deionized water, is stirred to dissolving, copperas solution solution is mixed with glucose solution, proceed to 100mL reactor, at being placed in 180 DEG C, baking oven, heat 24h.After heating, be cooled to room temperature, the sample of gained is washed, first use deionized water wash three times, then use washing with alcohol three times, then dry at 80 DEG C and spend the night.The sample of gained is calcined 5 ~ 6 hours at 550 DEG C, obtains caged ferric oxide hollow ball, to the present embodiment product (Fe
2o
3hollow ball) carry out scanning electron microscope to observe its microscopic appearance, result as shown in Figure 2, prepared Fe
2o
3sample is size uniform, and diameter is in the hollow ball shape structure of about 1000 ~ 1100nm, and the shell of ferric oxide is by 1 ~ 3 Fe
2o
3small-particle forms, and thickness is between 60 ~ 180nm.
Embodiment 3
5.88g ferrous ammonium sulphate is dissolved in 40mL deionized water, ultrasonic to dissolving completely.40g glucose is dissolved in 80mL deionized water, is stirred to dissolving, copperas solution solution is mixed with glucose solution, proceed to 100mL reactor, at being placed in 180 DEG C, baking oven, heat 24h.After heating, be cooled to room temperature, the sample of gained is washed, first use deionized water wash three times, then use washing with alcohol three times, then dry at 80 DEG C and spend the night.The sample of gained is calcined 5 ~ 6 hours at 550 DEG C, obtains caged ferric oxide hollow ball, to the present embodiment product (Fe
2o
3hollow ball) carry out scanning electron microscope to observe its microscopic appearance, result as shown in Figure 3, prepared Fe
2o
3sample is size uniform, and diameter is in the hollow ball shape structure of about 1400 ~ 1500nm, and the shell of ferric oxide is by 1 ~ 3 Fe
2o
3small-particle forms, and thickness is between 60 ~ 180nm.
Claims (6)
1. a preparation method for caged ferric oxide hollow ball, is characterized in that, comprises the following steps:
(1) ferrous ammonium sulphate is dissolved in deionized water, ultrasonic to dissolving completely;
(2) glucose is dissolved in deionized water;
(3) by the l ferrous ammonium sulfate solution of step (1) gained with mix in the glucose solution of step (2) gained after transfer in reactor, and be placed in baking oven and heat 22 ~ 26 hours at 160 ~ 200 DEG C, wherein the mol ratio of glucose and ferrous ion is 5-15:1;
(4) sample of step (3) gained cooled, wash, dry and spend the night;
(5) sample of step (4) gained is calcined 5 ~ 6 hours at 530 ~ 570 DEG C, obtain caged ferric oxide hollow ball.
2. the preparation method of a kind of caged ferric oxide hollow ball according to claim 1, is characterized in that: the volumetric molar concentration of described l ferrous ammonium sulfate solution is 0.2 ~ 0.5mol/L.
3. the preparation method of a kind of caged ferric oxide hollow ball according to claim 1, is characterized in that: the volumetric molar concentration of described glucose solution is 1.0 ~ 4.0mol/L.
4. the preparation method of a kind of caged ferric oxide hollow ball according to claim 1, is characterized in that: first use deionized water wash three times in described step (4), then uses washing with alcohol three times.
5. the preparation method of a kind of caged ferric oxide hollow ball according to claim 1, is characterized in that: in described step (4), bake out temperature is 70 ~ 90 DEG C.
6. adopt the caged ferric oxide hollow ball that as described in claim 1-5 any one prepared by method, it is characterized in that: size uniform, diameter is between 670 ~ 1500nm, and the shell thickness of ferric oxide is between 60 ~ 180nm.
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Cited By (2)
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CN106582621A (en) * | 2016-12-29 | 2017-04-26 | 杭州禹净环境科技有限公司 | Platinum-loaded hollowed-out titanium dioxide and preparation method thereof |
CN110961107A (en) * | 2019-12-10 | 2020-04-07 | 重庆工商大学 | Nano iron oxide material, preparation method and application thereof |
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CN102464304A (en) * | 2010-11-12 | 2012-05-23 | 中国科学院过程工程研究所 | Multi-shell-layer metal oxide hollow ball and preparation method thereof |
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US20130251624A1 (en) * | 2012-03-20 | 2013-09-26 | Korea University Research And Business Foundation | Method for preparation of hematite iron oxide with different nanostructures and hematite iron oxide prepared thereby |
CN105129864A (en) * | 2015-08-20 | 2015-12-09 | 电子科技大学 | Micron-order rugby-shaped iron oxide material and preparation method thereof |
-
2016
- 2016-01-15 CN CN201610028536.3A patent/CN105540681A/en active Pending
Patent Citations (4)
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CN102464304A (en) * | 2010-11-12 | 2012-05-23 | 中国科学院过程工程研究所 | Multi-shell-layer metal oxide hollow ball and preparation method thereof |
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Non-Patent Citations (4)
Title |
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DEJUAN DU ET AL.: "Ligand-Assisted Hydrothermal Synthesis of Hollow Fe2O3 Urchin-like Microstructures and Their Magnetic Properties", 《JOURNAL OF PHYSICAL CHEMISTRY C》 * |
JIAGUO YU ET AL.: "Hydrothermal Synthesis and Visible-light Photocatalytic Activity of Novel Cage-like Ferric Oxide Hollow Spheres", 《CRYSTAL GROWTH & DESIGN》 * |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106582621A (en) * | 2016-12-29 | 2017-04-26 | 杭州禹净环境科技有限公司 | Platinum-loaded hollowed-out titanium dioxide and preparation method thereof |
CN106582621B (en) * | 2016-12-29 | 2020-03-03 | 浙江光之媒新材料有限公司 | Hollow titanium dioxide loaded with metal platinum and preparation method thereof |
CN110961107A (en) * | 2019-12-10 | 2020-04-07 | 重庆工商大学 | Nano iron oxide material, preparation method and application thereof |
CN110961107B (en) * | 2019-12-10 | 2023-03-28 | 重庆工商大学 | Nano iron oxide material, preparation method and application thereof |
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Application publication date: 20160504 |