CN101041470A - Method for synthesizing block-shaped alpha-ferric oxide nanostructure - Google Patents
Method for synthesizing block-shaped alpha-ferric oxide nanostructure Download PDFInfo
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- CN101041470A CN101041470A CN 200710064685 CN200710064685A CN101041470A CN 101041470 A CN101041470 A CN 101041470A CN 200710064685 CN200710064685 CN 200710064685 CN 200710064685 A CN200710064685 A CN 200710064685A CN 101041470 A CN101041470 A CN 101041470A
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- ferric oxide
- alpha
- nano
- arginine
- iron trichloride
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000002086 nanomaterial Substances 0.000 title claims description 28
- 230000002194 synthesizing effect Effects 0.000 title 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 30
- ODKSFYDXXFIFQN-BYPYZUCNSA-N L-arginine Chemical compound OC(=O)[C@@H](N)CCCN=C(N)N ODKSFYDXXFIFQN-BYPYZUCNSA-N 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010189 synthetic method Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims description 29
- 229930064664 L-arginine Natural products 0.000 claims description 19
- 235000014852 L-arginine Nutrition 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 230000004087 circulation Effects 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 3
- 229910000831 Steel Inorganic materials 0.000 abstract description 2
- 239000010959 steel Substances 0.000 abstract description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract 1
- 229950000845 politef Drugs 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 31
- 239000002245 particle Substances 0.000 description 16
- 230000005540 biological transmission Effects 0.000 description 14
- 239000002105 nanoparticle Substances 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 229910000859 α-Fe Inorganic materials 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000004005 microsphere Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 229910001566 austenite Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000011858 nanopowder Substances 0.000 description 5
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000000696 magnetic material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000011246 composite particle Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 150000002505 iron Chemical class 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- 235000003891 ferrous sulphate Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 125000004103 aminoalkyl group Chemical group 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000003500 flue dust Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- -1 oxygenant Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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 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 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.
Description
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=0～4; Y 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-, 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 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 synthetic method of block alpha-ferric oxide nanostructure 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-, 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 blocky alpha-ferric oxide nanostructure.
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| CN102220638A (en) * | 2011-04-29 | 2011-10-19 | 中国科学院合肥物质科学研究院 | Preparation method of cubic iron trioxide monocrystal |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102220638A (en) * | 2011-04-29 | 2011-10-19 | 中国科学院合肥物质科学研究院 | Preparation method of cubic iron trioxide monocrystal |
| 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 |
| CN103028738A (en) * | 2012-12-26 | 2013-04-10 | 中北大学 | Method for controllably preparing FeNi3 micro-nano materials in various shapes |
| CN103028738B (en) * | 2012-12-26 | 2014-12-24 | 中北大学 | Method for controllably preparing FeNi3 micro-nano materials in various shapes |
| CN104229900A (en) * | 2014-09-15 | 2014-12-24 | 济南大学 | Preparation method of alpha-Fe2O3 cubes |
| 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 |
| 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 |
| CN106115792A (en) * | 2016-06-23 | 2016-11-16 | 兰州大学 | One prepares Fe with collagen protein for biomineralization template2o3the method of nanoparticle |
| 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 |
| CN112044456A (en) * | 2020-09-16 | 2020-12-08 | 合肥学院 | Ag3PO4/α-Fe2O3Preparation method and application of composite material |
| 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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