CN100491260C - Method for synthesizing block-shaped alpha-ferric oxide nanostructure - Google Patents

Method for synthesizing block-shaped alpha-ferric oxide nanostructure Download PDF

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CN100491260C
CN100491260C CNB2007100646856A CN200710064685A CN100491260C CN 100491260 C CN100491260 C CN 100491260C CN B2007100646856 A CNB2007100646856 A CN B2007100646856A CN 200710064685 A CN200710064685 A CN 200710064685A CN 100491260 C CN100491260 C CN 100491260C
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ferric oxide
arginine
alpha
nano
raw material
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CN101041470A (en
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曹化强
王国志
项军花
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Tsinghua University
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Tsinghua University
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Abstract

The invention discloses a synthetic method of lump alpha- ferric oxide nanometer structure, which comprises the following steps: making ferric chloride (FeCl3.6H2O), L- arginine (C6H14N4O2) as raw matThe invention discloses a synthetic method of lump alpha- ferric oxide nanometer structure, which comprises the following steps: making ferric chloride (FeCl3.6H2O), L- arginine (C6H14N4O2) as raw material; allocating ferric chloride and L- arginine water solution as reacting start liquid under room temperature; placing into rustless steel autoclave lining a politef; heating under 150-180 deg.c aterial; allocating ferric chloride and L- arginine water solution as reacting start liquid under room temperature; placing into rustless steel autoclave lining a politef; heating under 150-180 deg.c at 10-48 h; getting the product. This product use biomolecule--L-arginine as one of raw material, which possesses super material property and simple method. 10-48 h; getting the product. This product use biomolecule--L-arginine as one of raw material, which possesses super material property and simple method.

Description

A kind of synthetic method of block alpha-ferric oxide nanostructure
Technical field
The present invention relates to a kind of synthetic method of block alpha-ferric oxide nanostructure, belong to the preparing technical field of the semiconductor nano material of magnetic.
Background technology
Alpha-ferric oxide (α-Fe 2O 3) be n-N-type semiconductorN material, character such as the high-specific surface area of Nano semiconductor particles, high reactivity make it to become and are applied to the most promising material in transmitter aspect.In addition, alpha-ferric oxide also is the most stable at ambient temperature ferric oxide.At room temperature also have weak ferromagnetism, belong to half-hard magnetic material, can be applicable to rly., switch, semifixed storage, magnetic-light nano-device etc.No matter in academic research still in application facet, all have great importance.
By retrieval, there are 13 in the prior art about the alpha-iron oxide nano-powder patent report:
(1) " manufacture method of alpha-iron oxide nano-powder " (applicant: Ji'nan University, contriver: Li Ling; Application number 01130089), this disclosure of the Invention the manufacture method of different shapes alpha-iron oxide nano-powder, be characterized in that ferric ion solutions and basic solution react under the condition of introducing tensio-active agent, reaction is carried out at normal temperatures and pressures, adjust the proportioning of high and low molecular surface active agent, can obtain difform alpha-iron oxide nano-powder.The particle diameter of the ferric oxide powder of this method manufacturing reaches 10～30nm, and granularity is tiny evenly; Reaction is carried out at normal temperatures and pressures.
(2) " ferric oxide prepares nano dye and nano magnetic material ", (applicant: Shi Jiazhi, contriver: Shi Jiazhi, application number 02145680), this invention relates to a kind of iron and steel hot-work ferric oxide to prepare the technology of nano dye and nano magnetic material and processing method is to be that main raw material adds hydrochloric acid, sodium hydroxide, oxygenant, additive and carries out redox reaction and prepare nanometer iron oxide red, nano iron oxide yellow, nano-sized black iron oxide and nano magnetic material with the ferric oxide.
(3) " with the ferric oxide-organic composite granulated method for preparing the ferric oxide hollow particle of core/shell structure ", (applicant: Physical Chemistry Technology Inst., Chinese Academy of Sciences, the yellow loyal soldier of contriver: Tang Fangqiong, application number 03156712), this invention belongs to the technical field for preparing the inorganic hollow submicron particles with composite particles, and particularly usefulness (shell/nuclear) martial ethiops-organic complex microsphere prepares the method for magnetic hollow submicron particles.
(4) " preparation of ultra tiny ferric oxide ", (applicant: Chongqing City Chemical Engineering Inst., the contriver: flourish Wang De melts in the king, application number 87108286), this invention is the sulfur acid ferrous waste material to discharge in some Industrial processes, the treated ferrous sulfate crystal that obtains is a raw material, and the well-mixed solid state reaction of the carbonate of employing and basic metal or alkaline-earth metal is produced the method for ultra tiny ferric oxide.It comprises batch mixing, reaction, washes and dehydrates four technological processs.The maximum particle diameter of product is～100nm that minimum grain size is～8nm that median size is～36nm.
(5) " a kind of preparation method of super-fine nanometer ferric oxide powder ", (applicant: Weifujida New Material Application Development Co., Ltd., Wuxi, the contriver: Lu Jinshan Hang Sheng is big, application number 02112669.0), this invention relates to the preparation method of super-fine nanometer ferric oxide powder, belongs to field of fine chemical.Utilize cheap molysite industrial chemicals batch preparations ferric oxide (α-Fe 2O 3, γ-Fe 2O 3, Fe 3O 4) ultra-fine nano-powder, the grain-size of powder is disperseed near single, and its median size is respectively 10-20 nanometer (α-Fe 2O 3), 3-10 nanometer (γ-Fe 2O 3) and 5-15 nanometer (Fe 3O 4).
(6) " martial ethiops hollow microsphere particle and method for making and purposes " with meso-hole structure, (applicant: Physical Chemistry Technology Inst., Chinese Academy of Sciences, the yellow loyal soldier of contriver: Tang Fangqiong, application number 200310122436.X), this invention belongs to the technical field for preparing the inorganic hollow microsphere particle with composite particles, be particularly related to martial ethiops hollow particle, and use the martial ethiops hollow microsphere particulate method and the purposes of the mesoporous martial ethiops-organic composite granulated preparation meso-hole structure of core/shell structure with meso-hole structure.This invention is to use divalent iron salt solution control hydrolysis method to prepare mesoporous magnetic iron oxide particle it is coated on organic microballoons such as polystyrene, thereby obtains the mesoporous martial ethiops complex microsphere of core/shell structure.Adopt under slow temperature-rising method and the oxygen free condition organic core sintering in the uniform composite particles is fallen, the organic substance in the ferric oxide particles of shell also is sintered simultaneously, thereby obtains complete mesoporous martial ethiops hollow microsphere particle.
(7) " a kind of ultra-fine/preparation method of nano-sized iron oxide/iron powder ", (applicant: Central South University, contriver: model scape lotus Cheng Huichao, application number 200410023302.7), this invention relates to field of powder metallurgy, the method of the ultra-fine/nano-sized iron oxide that particularly adopts nanotechnology to prepare is characterized in that: adopt iron nitrate crystal (Fe (NO 3) 39H 2O), ferrous sulfate crystal (FeSO 47H 2O), iron(ic) chloride crystal (FeCl 36H 2O) be raw material, be mixed with the iron salt solutions of concentration for～30wt%; Adding ammoniacal liquor adjusting pH is 1.5～3; Add 0.1～1.0% tensio-active agent and 0.01～0.1% grain inhibitor again,, obtain transparent colloid through ultra-sonic oscillation 10～60min; Dry then, make ultra-fine mixed powder presoma; At 350～700 ℃ of temperature lower calcinations, obtain nanometer/superfine iron oxide powder.The powder size of the present invention's preparation is thin, and less than 100nm, the purity height reaches 99%～99.5%.
(8) " modified nano oxide compound, preparation method and its usage ", (applicant: Shanghai University Of Engineering Science, contriver: Shen Yong Qin Wei front yard Zhang Huifang king's fourth at dawn grain husk, application number 200410067399), this invention is a kind of modified nano oxide compound, preparation method and the purposes that is used for functional finishing agent.This modified nano oxide compound has following structural formula: suc as formula I wherein, A is a nano-oxide, and described nano-oxide is nano-titanium oxide, nano zine oxide, nano aluminium oxide, nano-sized iron oxide, nano silicon oxide and their mixture thereof; R=(CH 2/ n, N=0-4Y is vinyl, hydroxyl, aminoalkyl, amino, epoxy group(ing), methacryloyl oxyalkyl or sulfydryl; Suc as formula II wherein, m=0～20, R "=A, H and C 1-4Alkyl.System makes after by the reaction of nano-oxide and properties-correcting agent, emulsification.
(9) " PREPARATION OF NANO FERRIC OXIDE method ", (applicant: Shanghai University, the red clock of the positive Wu Ming of contriver: Li Zhenjiao sea warship Lv Senlin, application number 200510023582), this invention relates to a kind of PREPARATION OF NANO FERRIC OXIDE method, particularly a kind of method that adopts the electron beam irradiation legal system to be equipped with nano-sized iron oxide.
(10) " iron oxide sensitized lamellar titanium oxide visible light catalyst and preparation method, " (applicant: Shanghai Silicate Inst., Chinese Academy of Sciences, the contriver: high Lian Liu Hong is gorgeous, application number 200510023961), this invention provides low-gap semiconductor α-Fe 2O 3The nano-titanium oxide light sheets catalyzer of sensitization and original position synthetic preparation method.
(11) " a kind of preparation method of magnetic ferric oxide nano particles ", (applicant: East China Normal University, the contriver: Jiang Ji Sen Jiang state Hua Ding builds virtue, application number 200510111203.9), this invention relates to a kind of preparation method of magnetic ferric oxide nano particles, belongs to the technical field of inorganic nonmetal magnetic nano material preparation.This invention utilizes special organic additive and inorganic salt at γ-Fe 2O 3Effect in the crystal formation process is a raw material with the trivalent iron salt, must not pass through redox processes, directly prepares length-to-diameter ratio at a lower temperature and be bar-shaped γ-Fe of 6 2O 3Nanoparticle and particle diameter are cube γ-Fe of 20nm 2O 3Nanoparticle.The present invention has the advantages that technological process is simple, particle shape is easy to control.
(12) " a kind of synthetic method of alpha-ferric oxide nano particle of American football shape, applicant: Cao Huaqiang, Zhang Lei, application number: 200610002148.4), this invention relates to a kind of preparation technology of semiconductor nano material.
(13) " PREPARATION OF NANO FERRIC OXIDE method and apparatus ", (applicant: Tianyi Superfine Metal Powders Co., Ltd., Jiangsu, the contriver: height is prosperous Zhang Lili, application number 200610037674.4), this invention relates to a kind of PREPARATION OF NANO FERRIC OXIDE technology and equipment thereof, with pentacarbonyl iron or its steam pressurization N 2Or the rare gas element band carries, and makes under its pressure more than 0.01Mpa the raw material pipeline nozzle atomization ejection in the reactor, carries out combustion reactions with the oxygen or the air of the ejection of gas pipeline nozzle in reactor; The iron oxide particles of combustion reactions falls into the liquid sedimentation medium in the reactor, so that each iron oxide particles that generates is isolated by sedimentation liquid; The reception of combustion reactions resultant after the sedimentation, oven dry, cooling are obtained the nano-sized iron oxide finished product.Its equipment used feature is that reactor comprises combustion chamber, settling pocket, receptor, flue dust chamber, and cooling room is looped around the outside of reactor, and this invention gained nano-sized iron oxide has good color and dispersiveness, makes that color is dark and tinting strength is high, applied range.
Summary of the invention
The object of the present invention is to provide the hydrothermal synthesis method of the blocky alpha-ferric oxide nanostructure of a kind of easy preparation.Raw materials used being easy to get in the synthetic method of the present invention, technology is easy, can synthesize the blocky alpha-ferric oxide nanostructure of size and dimension than homogeneous.
The synthetic method of a kind of block alpha-ferric oxide nanostructure that the present invention proposes is characterized in that this method is carried out as follows:
(1) with iron trichloride (FeCl 36H 2O), L-arginine (C 6H 14N 4O 2) be raw material, at room temperature, preparation comprises iron trichloride, the arginic aqueous solution of L-, wherein the iron trichloride concentration range is 0.270 3/ 40 milliliters of～0.8019 grams, L-arginine concentration range are/40 milliliters of 0.1742～4.7024 grams;
(2) described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 150～180 ℃ of temperature range heating 10～48 hours;
(3) throw out that obtains after will reacting washs three circulations successively through deionized water and washing with alcohol, puts into loft drier then and carries out drying 2 hours for 80 ℃, promptly obtains blocky alpha-ferric oxide nanostructure.
Because character and its size, shape and the reaction system of nano material have much relations, a kind of alpha-ferric oxide nanostructure that the present invention synthesizes is to utilize biomolecules---the L-arginine is that one of raw material participates in reaction, therefore, synthetic method is simple, material property is good, is suitable for commercial application.
Description of drawings
Fig. 1: (a) being the transmission electron microscope photo of embodiment 1, (b) is the X-ray diffractogram of embodiment 1.
Fig. 2: (a) being the transmission electron microscope photo of embodiment 2, (b) is the X-ray diffractogram of embodiment 2.
Fig. 3: (a) being the transmission electron microscope photo of embodiment 3, (b) is the X-ray diffractogram of embodiment 3.
Fig. 4: (a) being the transmission electron microscope photo of embodiment 4, (b) is the X-ray diffractogram of embodiment 4.
Fig. 5: (a) being the transmission electron microscope photo of embodiment 5, (b) is the X-ray diffractogram of embodiment 5.
Fig. 6: (a) being the transmission electron microscope photo of embodiment 6, (b) is the X-ray diffractogram of embodiment 6.
Fig. 7: (a) being the transmission electron microscope photo of embodiment 7, (b) is the X-ray diffractogram of embodiment 7.
Embodiment
Below by specific embodiment the present invention further is illustrated.
Embodiment 1:
---with iron trichloride (FeCl 36H 2O), L-arginine (C 6H 14N 4O 2) be raw material, at room temperature, preparation comprises iron trichloride, the arginic aqueous solution of L-, and wherein iron trichloride concentration is/40 milliliters of 0.2703 grams, and L-arginine concentration is/40 milliliters of 0.1742 grams.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, and heating is 10 hours under 180 ℃ of temperature.
---the throw out that will obtain after will reacting washs three circulations successively through deionized water and washing with alcohol, puts into loft drier (80 ℃) then and carries out drying 2 hours, promptly obtains blocky alpha-ferric oxide nanostructure.
Fig. 1 (a) is the x-ray diffraction pattern of embodiment 1, determines that product is an alpha-ferric oxide, and Fig. 1 (b) is the transmission electron microscope photo of blocky alpha-ferric oxide nanostructure, and its length of side on average is about 210 nanometers as seen from the figure.
Embodiment 2:
---with iron trichloride (FeCl 36H 2O), L-arginine (C 6H 14N 4O 2) be raw material, at room temperature, preparation comprises iron trichloride, the arginic aqueous solution of L-, and wherein iron trichloride concentration is/40 milliliters of 0.8109 grams, and L-arginine concentration is/40 milliliters of 0.5226 grams.
Described mixing solutions is positioned in the teflon-lined stainless steel cauldron, and heating is 10 hours under 180 ℃ of temperature.
---the throw out that will obtain after will reacting washs three circulations successively through deionized water and washing with alcohol, puts into loft drier (80 ℃) then and carries out drying 2 hours, promptly obtains blocky alpha-ferric oxide nanostructure.
Fig. 2 (a) is the x-ray diffraction pattern of embodiment 2, determines that product is an alpha-ferric oxide, and Fig. 2 (b) is the transmission electron microscope photo of blocky alpha-ferric oxide nanostructure, and its length of side on average is about 846 nanometers as seen from the figure.
Embodiment 3:
---with iron trichloride (FeCl 36H 2O), L-arginine (C 6H 14N 4O 2) be raw material, at room temperature, preparation comprises iron trichloride, the arginic aqueous solution of L-, and wherein iron trichloride concentration is/40 milliliters of 0.8109 grams, and L-arginine concentration is/40 milliliters of 1.5678 grams.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, and heating is 10 hours under 180 ℃ of temperature.
---the throw out that will obtain after will reacting washs three circulations successively through deionized water and washing with alcohol, puts into loft drier (80 ℃) then and carries out drying 2 hours, promptly obtains blocky alpha-ferric oxide nanostructure.
Fig. 3 (a) is the x-ray diffraction pattern of embodiment 3, determines that product is an alpha-ferric oxide, and Fig. 3 (b) is the transmission electron microscope photo of blocky alpha-ferric oxide nanostructure, and its length of side on average is about 597 nanometers as seen from the figure.
Embodiment 4:
---with iron trichloride (FeCl 36H 2O), L-arginine (C 6H 14N 4O 2) be raw material, at room temperature, preparation comprises iron trichloride, the arginic aqueous solution of L-, and wherein iron trichloride concentration is/40 milliliters of 0.8109 grams, and L-arginine concentration is/40 milliliters of 1.5678 grams.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, and heating is 24 hours under 180 ℃ of temperature.
---the throw out that will obtain after will reacting washs three circulations successively through deionized water and washing with alcohol, puts into loft drier (80 ℃) then and carries out drying 2 hours, promptly obtains blocky alpha-ferric oxide nanostructure.
Fig. 4 (a) is the x-ray diffraction pattern of embodiment 4, determines that product is an alpha-ferric oxide, and Fig. 4 (b) is the transmission electron microscope photo of blocky alpha-ferric oxide nanostructure, and its length of side on average is about 491 nanometers as seen from the figure.
Embodiment 5:
---with iron trichloride (FeCl 36H 2O), L-arginine (C 6H 14N 4O 2) be raw material, at room temperature, preparation comprises iron trichloride, the arginic aqueous solution of L-, and wherein iron trichloride concentration is/40 milliliters of 0.8109 grams, and L-arginine concentration is/40 milliliters of 4.7024 grams.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, and heating is 24 hours under 180 ℃ of temperature.
---the throw out that will obtain after will reacting washs three circulations successively through deionized water and washing with alcohol, puts into loft drier (80 ℃) then and carries out drying 2 hours, promptly obtains blocky alpha-ferric oxide nanostructure.
Fig. 5 (a) is the x-ray diffraction pattern of embodiment 5, determines that product is an alpha-ferric oxide, and Fig. 5 (b) is the transmission electron microscope photo of blocky alpha-ferric oxide nanostructure, and its length of side on average is about 54 nanometers as seen from the figure.
Embodiment 6:
---with iron trichloride (FeCl 36H 2O), L-arginine (C 6H 14N 4O 2) be raw material, at room temperature, preparation comprises iron trichloride, the arginic aqueous solution of L-, and wherein iron trichloride concentration is/40 milliliters of 0.8109 grams, and L-arginine concentration is/40 milliliters of 4.7024 grams.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, and heating is 48 hours under 180 ℃ of temperature.
---the throw out that will obtain after will reacting washs three circulations successively through deionized water and washing with alcohol, puts into loft drier (80 ℃) then and carries out drying 2 hours, promptly obtains blocky alpha-ferric oxide nanostructure.
Fig. 6 (a) is the x-ray diffraction pattern of embodiment 6, determines that product is an alpha-ferric oxide, and Fig. 6 (b) is the transmission electron microscope photo of blocky alpha-ferric oxide nanostructure, and its length of side on average is about 64 nanometers as seen from the figure.
Embodiment 7:
---with iron trichloride (FeCl 36H 2O), L-arginine (C 6H 14N 4O 2) be raw material, at room temperature, preparation comprises iron trichloride, the arginic aqueous solution of L-, and wherein iron trichloride concentration is/40 milliliters of 0.8109 grams, and L-arginine concentration is/40 milliliters of 1.5678 grams.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, and heating is 10 hours under 150 ℃ of temperature.
---the throw out that will obtain after will reacting washs three circulations successively through deionized water and washing with alcohol, puts into loft drier (80 ℃) then and carries out drying 2 hours, promptly obtains blocky alpha-ferric oxide nanostructure.
Fig. 7 (a) is the x-ray diffraction pattern of embodiment 7, determines that product is an alpha-ferric oxide, and Fig. 7 (b) is the transmission electron microscope photo of blocky alpha-ferric oxide nanostructure, and its length of side on average is about 591 nanometers as seen from the figure.

Claims (1)

1, a kind of block alpha-ferric oxide synthetic method of nanostructure is characterized in that this method is carried out as follows:
(1) be raw material with iron trichloride, L-arginine, at room temperature, preparation comprises iron trichloride, the arginic aqueous solution of L-, and wherein the iron trichloride concentration range is/40 milliliters of 0.2703～0.8019 grams, and L-arginine concentration range is/40 milliliters of 0.1742～4.7024 grams;
(2) described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 150～180 ℃ of temperature range heating 10～48 hours;
(3) throw out that obtains after will reacting washs three circulations successively through deionized water and washing with alcohol, puts into loft drier then and carries out drying 2 hours for 80 ℃, promptly obtains the block alpha-ferric oxide of nanostructure.
CNB2007100646856A 2007-03-23 2007-03-23 Method for synthesizing block-shaped alpha-ferric oxide nanostructure Expired - Fee Related CN100491260C (en)

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CN102220638B (en) * 2011-04-29 2013-02-13 中国科学院合肥物质科学研究院 Preparation method of cubic iron trioxide monocrystal
CN103028738B (en) * 2012-12-26 2014-12-24 中北大学 Method for controllably preparing FeNi3 micro-nano materials in various shapes
CN104229900B (en) * 2014-09-15 2015-12-30 济南大学 A kind of α-Fe 2o 3the preparation method of cubic block
CN104445428A (en) * 2014-11-04 2015-03-25 华文蔚 Synthesis method of spark plasma sintered massive alpha-ferric oxide
CN105129864B (en) * 2015-08-20 2017-01-11 电子科技大学 Micron-order rugby-shaped iron oxide material and preparation method thereof
CN106115792B (en) * 2016-06-23 2018-08-17 兰州大学 One kind preparing Fe by biomineralization template of collagen2O3The method of nano-particle
CN112044456B (en) * 2020-09-16 2022-06-21 合肥学院 Ag3PO4/α-Fe2O3Preparation method and application of composite material

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