CN105540681A - Cage-shaped ferric oxide hollow ball and preparation method thereof - Google Patents

Cage-shaped ferric oxide hollow ball and preparation method thereof Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
ferric oxide
hollow ball
oxide hollow
preparation
caged
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610028536.3A
Other languages
Chinese (zh)
Inventor
司崇殿
孔苗苗
刘广军
高洪涛
戴冬梅
孙玉红
韩红
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jining University
Original Assignee
Jining University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jining University filed Critical Jining University
Priority to CN201610028536.3A priority Critical patent/CN105540681A/en
Publication of CN105540681A publication Critical patent/CN105540681A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide [Fe2O3]
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • C01P2004/34Spheres 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

A kind of caged ferric oxide hollow ball and preparation method thereof
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.
CN201610028536.3A 2016-01-15 2016-01-15 Cage-shaped ferric oxide hollow ball and preparation method thereof Pending CN105540681A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610028536.3A CN105540681A (en) 2016-01-15 2016-01-15 Cage-shaped ferric oxide hollow ball and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610028536.3A CN105540681A (en) 2016-01-15 2016-01-15 Cage-shaped ferric oxide hollow ball and preparation method thereof

Publications (1)

Publication Number Publication Date
CN105540681A true CN105540681A (en) 2016-05-04

Family

ID=55820316

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610028536.3A Pending CN105540681A (en) 2016-01-15 2016-01-15 Cage-shaped ferric oxide hollow ball and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105540681A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
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
CN110961107A (en) * 2019-12-10 2020-04-07 重庆工商大学 Nano iron oxide material, preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102824884A (en) * 2012-05-14 2012-12-19 无锡润鹏复合新材料有限公司 TiO2/Fe2O3 composite hollow microsphere and preparation method thereof
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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
CN102824884A (en) * 2012-05-14 2012-12-19 无锡润鹏复合新材料有限公司 TiO2/Fe2O3 composite hollow microsphere and preparation method thereof
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

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
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》 *
SHUBO WANG ET AL.: "Hollow a-Fe2O3 Nanospheres Synthesized Using a Carbon Template as Novel Anode Materials for Na-Ion Batteries", 《CHEMELECTROCHEM COMMUNICATIONS》 *
关雨豪: "水热法合成多孔纳米Fe2O3气敏材料", 《中国优秀硕士学位论文全文数据库 工程科技Ι辑》 *

Cited By (4)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
CN109133193B (en) Method for preparing metal hydroxide multilevel structure by utilizing MOF derived bimetallic oxide template
WO2019109831A1 (en) Method for preparing copper-nickel cobaltate nanowires and use thereof in catalyzing hydrolysis of ammonia borane to produce hydrogen
CN103708551B (en) The preparation method of a kind of ethylene glycol-water mixed solvent thermal synthesis bismuth oxycarbonate flower-like microsphere
CN103537237B (en) A kind of Fe 3o 4the preparation method of CPAM core-shell magnetic nano material
CN102824884B (en) A kind of TiO 2/ Fe 2o 3compound hollow microballoon and preparation method thereof
CN109205567B (en) Method for preparing metal oxide multilevel structure by utilizing MOF derived bimetallic oxide template
CN103771485B (en) A kind of controllable method for preparing of cupric oxide three-dimensional manometer self-assembly
CN103818954B (en) The anatase octahedrite TiO of face exposure that one has (001) 2the preparation method of tiny balloon
CN105384192B (en) Method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5
CN103539210A (en) Preparation method of cobalt molybdate microcrystals
CN102050479A (en) Ceric oxide nanorod and preparation method thereof
CN106542560B (en) A kind of preparation method of rare earth oxysulfate
CN111115694B (en) Preparation method of hollow Co-Fe LDH material
CN109879312A (en) A kind of preparation method of photocatalyst of titanium dioxide nano-powder
CN104671289B (en) A kind of Fe2O3Nanometer sheet and preparation method thereof
CN104439276B (en) A kind of quick method and product preparing hollow porous silica/argentum nano composite material
CN103663562A (en) Method for low-temperature preparation of nano bismuth tungstate
CN105129849A (en) Flowerlike nano-sized titanium dioxide material and template-free preparation method thereof
CN104971703A (en) Preparation method of polypyrrole coated magnetic reduced graphene nanometer material
CN105540681A (en) Cage-shaped ferric oxide hollow ball and preparation method thereof
CN102502871B (en) Method for synthesizing three-dimensional porous ferric oxide nano rod cluster
CN105565375A (en) Preparing method for nanoscale porous titanium dioxide hollow spheres
CN105585035A (en) Preparation method of alumina hollow microspheres
CN103833086A (en) Preparation method of flaky iron trioxide
CN101343043B (en) Amphoteric metal compound nano-material and method of preparing the same

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20160504