CN105129862A - Preparation method and applications of rice-grain-like nanometer magnetic iron oxide - Google Patents
Preparation method and applications of rice-grain-like nanometer magnetic iron oxide Download PDFInfo
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- CN105129862A CN105129862A CN201510480659.6A CN201510480659A CN105129862A CN 105129862 A CN105129862 A CN 105129862A CN 201510480659 A CN201510480659 A CN 201510480659A CN 105129862 A CN105129862 A CN 105129862A
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 35
- 235000009566 rice Nutrition 0.000 claims abstract description 35
- 235000013339 cereals Nutrition 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 241000209094 Oryza Species 0.000 claims description 34
- 239000008187 granular material Substances 0.000 claims description 17
- -1 iron carbonyl oxide compound Chemical class 0.000 claims description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001069 Raman spectroscopy Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 claims description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- 239000000047 product Substances 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 5
- 230000005415 magnetization Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 abstract 3
- 238000003760 magnetic stirring Methods 0.000 abstract 2
- 240000007594 Oryza sativa Species 0.000 abstract 1
- 238000009826 distribution Methods 0.000 abstract 1
- 150000002505 iron Chemical class 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 24
- 239000002105 nanoparticle Substances 0.000 description 16
- 239000002131 composite material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- JBPWDTQELHPIPV-UHFFFAOYSA-N n-(3,6-dihydro-2h-pyridin-1-yl)pyridine-4-carboxamide Chemical compound C=1C=NC=CC=1C(=O)NN1CCC=CC1 JBPWDTQELHPIPV-UHFFFAOYSA-N 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 229920001469 poly(aryloxy)thionylphosphazene Polymers 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000007669 thermal treatment Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910003153 β-FeOOH Inorganic materials 0.000 description 2
- WCDSVWRUXWCYFN-UHFFFAOYSA-N 4-aminobenzenethiol Chemical compound NC1=CC=C(S)C=C1 WCDSVWRUXWCYFN-UHFFFAOYSA-N 0.000 description 1
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002110 nanocone Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000000479 surface-enhanced Raman spectrum Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000004304 visual acuity Effects 0.000 description 1
Landscapes
- Compounds Of Iron (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The present invention discloses a preparation method of a rice-grain-like nanometer magnetic iron oxide. The preparation method comprises: respectively dissolving an iron salt and an anionic surfactant in deionized water, stirring to obtain a transparent solution, carrying out a mixing reaction on the two solutions, and carrying out magnetic stirring; carrying out centrifugation separation on the reaction solution, removing the supernatant, washing, and drying to obtain a rice-grain-like hydroxyl iron oxide; and carrying out a heat treatment on the rice-grain-like hydroxyl iron oxide at a certain temperature in a certain atmosphere so as to obtain the rice-grain-like nanometer magnetic iron oxide. According to the present invention, the rice-grain-like hydroxyl iron oxide having the uniform structure is obtained through magnetic stirring, and the nanometer magnetic iron oxide having the perfect rice grain shape is prepared through different heat treatments; and the method is simple and is easy to perform, the production cost is low, the controllability is strong, the aspect ratio of the rice-grain-like iron oxide can be controlled, and the obtained product has characteristics of narrow distribution, high yield, high purity and high saturation magnetization.
Description
Technical field
The invention belongs to ferriferous oxide preparation field, relate to a kind of preparation method of ferriferous oxide, specifically a kind of preparation method of rice-granule nano magnetic iron oxide and application.
Background technology
Ferriferous oxide mainly comprises Fe
20
3and Fe
30
4the ferriferous oxide nano composite material of various pattern is because of the physicochemical property with uniquenesses such as small-size effect, surface effects, synergistic effects, and the feature of easy functionalization, there is fine application prospect, cause in catalytic field, biomedical sector and cosmetic field, military field, new forms of energy etc. and pay close attention to widely.
As everyone knows, the character of ferriferous oxide determines its application.And the character of particle depends primarily on its size, pattern and structure, wherein morphology of particles and pattern are two the most key influence factors, therefore, the structure of nano material and morphology control research become one of the forward position and focus of present material scientific research.And synthesis has anisotropic Magnetic Nanocrystals Containing, not only contribute to understanding nanocrystalline process of growth, also help the magnetic property of the uniqueness obtained due to the generation of pattern anisotropy.Under usual conditions, along with the change of the length-to-diameter ratio of one dimension particle, the coercive force of particle also can change, and therefore controls the magneticsubstance that synthesis has different length-to-diameter ratio, contributes to the range of application widening ferriferous oxide.Up to the present, to have adopted various physico-chemical process to prepare monodispersed has the anisotropic ferriferous oxide nano material of pattern for people, as spherical, octahedra, nano wire, nano chain, nano belt, nanotube, nano-cone array, the nanostructure such as nano-hollow ball and nano flower [1-6] (reference: [1] WuW, XiaoXH, ZhangSF, LiH, ZhouXD, JiangCZ.One-potreactionandsubsequentannealingtosynthesis hollowsphericalmagnetiteandmaghemitenanocages.NanoscaleR es.Lett., 2009, 4:926. [2] PitzschelK, MorenoJMM, EscrigJ, AlbrechtO, NielschK, BachmannJ.Controlledintroductionofdiametermodulationsina rrayedmagneticironoxidenanotubes.ACSNano, 2009, 3:3463. [3] FanHM, YouGJ, LiY, ZhengZ, TanHR, ShenZX, TangSH, FengYP.Shape-controlledsynthesisofsingle-crystallineFe2O 3hollownanocrystalsandtheirtunableopticalproperties.J.Ph ys.Chem.C., 2009, 113:9928. [4] OmiS, KanetakaA, ShimamoriY, SupsakulchaiA, NagaiM, MaGH.Magnetite (Fe3O4) microcapsulespreparedusingaglassmembraneandsolventremova l.J.Microencapsule., 2001, 18:749. [5] MandalS, MullerAHE.Facileroutetothesynthesisofporousalpha-Fe2O3na norods.Mater.Chem.Phys., 2008, 111:438. [6] WuW, XiaoXH, ZhangSF, FanLX, PengTC, RenF, JiangCZ.Facilefabricationofultrafinehollowsilicaandmagne tichollowsilicananoparticlesbyadual-templatingapproach.N anoscaleRes.Lett., 2010, 5:116.).And for constructing comparatively big L/D ratio ferriferous oxide, especially have monodispersity, well-crystallized the report of grain of rice shape iron oxide nanoparticle aspect relatively less.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of rice-granule nano magnetic iron oxide, the method low in raw material price, operation steps are simple, and the grain of rice shape magnetic iron oxide of gained is stablized, have good magnetic, recoverable, can also be used as desirable surface reinforced Raman active base material model.
Object of the present invention can be achieved through the following technical solutions:
A preparation method for rice-granule nano magnetic iron oxide, is characterized in that, comprises the following steps:
(1) respectively molysite and anion surfactant are dissolved in deionized water, stir and obtain clear solution, then by two kinds of solution hybrid reactions, magnetic agitation;
(2) by the reaction solution centrifugation that step (1) obtains, remove supernatant liquor, washing, drying, obtain grain of rice shape iron carbonyl oxide compound;
(3) grain of rice shape iron carbonyl oxide compound step (2) obtained is heat-treated in the certain atmosphere of certain temperature, namely obtains rice-granule nano magnetic iron oxide.
As preferred further, in step of the present invention (1), molysite is the one in FERRIC CHLORIDE ANHYDROUS, Iron(III) chloride hexahydrate, ferric sulfate, iron nitrate.
As preferred further, in step of the present invention (1), anion surfactant is the one in cetyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, Trimethyllaurylammonium bromide, Sodium dodecylbenzene sulfonate.
As preferred further, in step of the present invention (1), the mol ratio of anion surfactant and molysite is 0 ~ 2.
As preferred further, in step of the present invention (1), the hybrid reaction time is 40-100 DEG C, and the reaction times is 2-12h.
As preferred further, in step of the present invention (3), heat treated temperature is 200-450 DEG C, and heat treatment time is 1-4h, and heat treated atmosphere is vacuum or hydrogen.
As further preferably, in step of the present invention (2), washing step is: first with deionized water by product cleaning 3 times, then use absolute ethanol washing, centrifugal; Described drying is 50 DEG C of dried overnight.
The present invention is the openly application of rice-granule nano magnetic iron oxide in surface reinforced Raman active base material also.
The present invention can regulate the length-to-diameter ratio of grain of rice shape hydrous iron oxide to change between 8:1 ~ 3:1 by the consumption and kind controlling anion surfactant and molysite.
Beneficial effect of the present invention: the preparation method of rice-granule nano magnetic iron oxide of the present invention obtains the grain of rice shape hydrous iron oxide with homogeneous structural by magnetic agitation, has perfect rice-granule nano magnetic iron oxide by different thermal treatment is obtained; The inventive method simple possible, production cost is low, Modulatory character is strong, the length-to-diameter ratio of controlled rice milling granular iron oxide compound, products therefrom narrowly distributing, output is high, purity is high, saturation magnetization is high, thus embodies important application prospect in fields such as magnetic recording material, catalyzer, biomedical sector, Magnetic resonance imaging, environment measurings.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph (SEM) of rice granulated samples prepared by the embodiment of the present invention 1: a is the stereoscan photograph of grain of rice shape hydrous iron oxide, and b is the stereoscan photograph of grain of rice shape ferriferous oxide.
Fig. 2 is the X-ray diffractogram of grain of rice shape hydrous iron oxide prepared by the embodiment of the present invention 1.
Fig. 3 is the Fe that the embodiment of the present invention 3 prepares
3o
4the X-ray diffractogram of nanoparticle.
Fig. 4 is that the embodiment of the present invention 3 prepares Fe
3o
4the magnetic hysteresis loop figure of nanoparticle.
Fig. 5 is grain of rice shape Fe of the present invention
3o
4the surface enhanced Raman spectroscopy figure ofAu composite nanostructure.
Embodiment
For the ease of it will be appreciated by those skilled in the art that the present invention is further illustrated below in conjunction with accompanying drawing.
embodiment 1
Hydrolysis method is adopted to prepare hydrous iron oxide.
By anhydrous FeCl
3be dissolved in 30mL deoxidation ionized water respectively with palmityl trimethyl ammonium chloride, stir and obtain clear solution, obtain FeCl
3concentration be 0.1mol/L, the concentration of palmityl trimethyl ammonium chloride is 0.05mol/L.Then by two kinds of solution mixing, at 40 DEG C of magnetic agitation 12h, react complete, by the centrifugation of gained reaction solution, remove supernatant liquor, spend oxonium ion water again and clean three times, then use absolute ethanol washing, centrifugal, 50 DEG C of dried overnight, the length-to-diameter ratio finally obtaining grain of rice shape is the yellow hydrous iron oxide of 4:1.
By above-mentioned gained hydrous iron oxide calcination 4h in 200 DEG C of vacuum, obtaining red grain of rice shape length-to-diameter ratio is the Fe of 4:1
2o
3nanoparticle.
Fig. 1 is the stereoscan photograph of rice granulated samples prepared by the embodiment of the present invention 1: a is the stereoscan photograph of grain of rice shape hydrous iron oxide, and b is the stereoscan photograph of grain of rice shape ferriferous oxide.As can be seen from two pictures contrasts, before and after thermal treatment, the pattern of sample is grain of rice shape, and grain of rice shape Fe2O3 length is about 300nm, and diameter is about 75nm, size uniformity, presents good dispersiveness.Fig. 2 is the X-ray diffractogram of grain of rice shape hydrous iron oxide prepared by the embodiment of the present invention 1, corresponding consistent with the standard card 34-1266 of β-FeOOH, does not have other assorted peaks, illustrate that the sample obtained is the β-FeOOH of pure phase, and crystalline structure is fine.
embodiment 2
Hydrolysis method is adopted to prepare hydrous iron oxide.
By Fe
2(SO
4)
3be dissolved in 30mL deoxidation ionized water respectively with Sodium dodecylbenzene sulfonate, stir and obtain clear solution, obtain Fe
2(SO
4)
3concentration be 0.2mol/L, the concentration of Sodium dodecylbenzene sulfonate is 0.15mol/L.Then by two kinds of solution mixing, 4h is stirred at 80 DEG C of condition lower magnetic forces.React complete, by the centrifugation of gained reaction solution, remove supernatant liquor, then spend oxonium ion water product cleaning three times, then use absolute ethanol washing, centrifugal, 50 DEG C of dried overnight, the length-to-diameter ratio finally obtaining grain of rice shape is the yellow hydrous iron oxide of 8:1.
By above-mentioned gained hydrous iron oxide calcination 3h in 300 DEG C of vacuum, obtaining red grain of rice shape length-to-diameter ratio is the Fe of 8:1
2o
3nanoparticle.
embodiment 3
Hydrolysis method is adopted to prepare hydrous iron oxide.
By FeCl
36H
2o and Trimethyllaurylammonium bromide are dissolved in 30mL deoxidation ionized water respectively, stir and obtain clear solution, obtain FeCl
36H
2the concentration of O is 0.1mol/L, and the concentration of Trimethyllaurylammonium bromide is 0.2mol/L.Then by two kinds of solution mixing, 10h is stirred at 50 DEG C of condition lower magnetic forces.React complete, by the centrifugation of gained reaction solution, remove supernatant liquor, then spend oxonium ion water product cleaning three times, then use absolute ethanol washing, centrifugal, 50 DEG C of dried overnight, the length-to-diameter ratio finally obtaining yellow grain of rice shape is the hydrous iron oxide of 6:1.
By above-mentioned gained hydrous iron oxide calcination 2h in 400 DEG C of hydrogen, obtaining black grain of rice shape length-to-diameter ratio is the Fe of 6:1
3o
4nanoparticle.
Fig. 3 is the Fe that the embodiment of the present invention 3 prepares
3o
4the X-ray diffractogram of nanoparticle, with Fe
3o
4standard card 01-1111 corresponding consistent, there is no other assorted peaks, illustrate that the sample that thermal treatment obtains is the Fe of pure phase
3o
4, and crystalline structure is fine.
Fig. 4 is that the embodiment of the present invention 3 prepares Fe
3o
4the magnetic hysteresis loop figure of nanoparticle, grain of rice shape Fe
3o
4present the magnetic property of superparamagnetism, and magnetic saturation intensity is about 87emu/g, there is higher magnetic responsiveness.
embodiment 4
Hydrolysis method is adopted to prepare hydrous iron oxide.
By Fe (NO
3)
3be dissolved in 30mL deoxidation ionized water respectively with cetyl trimethylammonium bromide, stir and obtain clear solution, obtain Fe (NO
3)
3concentration be 0.1mol/L, the concentration of cetyl trimethylammonium bromide is 0mol/L.Then by two kinds of solution mixing, 6h is stirred at 100 DEG C of condition lower magnetic forces.React complete, by the centrifugation of gained reaction solution, remove supernatant liquor, then spend oxonium ion water product cleaning three times, then use absolute ethanol washing, centrifugal, 50 DEG C of dried overnight, the length-to-diameter ratio finally obtaining yellow grain of rice shape is the hydrous iron oxide of 3:1.
By above-mentioned gained hydrous iron oxide calcination 1h in 450 DEG C of hydrogen, obtaining black grain of rice shape length-to-diameter ratio is the Fe of 3:1
3o
4nanoparticle.
Embodiment 5
With embodiment 3 gained grain of rice shape Fe
3o
4nanoparticle, grafting Au particle, tests its surface reinforced Raman active.
Get 10mg embodiment 3 gained grain of rice shape Fe
3o
4nanoparticle, is first undertaken functionalized by 3-aminopropyl trimethoxy siloxane, then it is mixed with 20mLAu nanoparticle, after fully assembling, product magnet is collected and is dissolved in 1mL deionized water, then adds 10mL deionized water, 2mL1% sodium citrate solution and 1mL0.1M oxammonium hydrochloride.Then, 1mL1%HAuCl
4dropwise join in above-mentioned solution under vibration, until the end of reduction process, product magnet is collected and is cleaned, obtained grain of rice shape Fe
3o
4Au composite nanoparticle.
With the Fe obtained under this condition
3o
4Au composite nanoparticle, as surface-enhanced Raman spectrum active substrate, drips the p-Mercaptoaniline (PATP) of 20 μ L different concns respectively, after drying, surveys its Raman signal, obtain surface enhanced Raman spectroscopy figure, as shown in Figure 5.With grain of rice shape Fe
3o
4Au composite nanoparticle is as substrate, and PATP is the Raman spectrogram of probe molecule, is 1 × 10 in PATP concentration
-7during M, still have very strong SERS signal, can meet the testing requirement of national standard to contaminant trace species, in spectrogram, the signal of PATP is detailed, and resolving power is very high.The grain of rice shape Fe that the present invention obtains
3o
4Au composite nanoparticle is as SERS substrate, and signal is even, and favorable repeatability, detection sensitivity is high, can be used for the detection of environmental pollutant and biomolecules.
Above content is only to structure example of the present invention and explanation; affiliated those skilled in the art make various amendment to described specific embodiment or supplement or adopt similar mode to substitute; only otherwise depart from the structure of invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
Claims (8)
1. a preparation method for rice-granule nano magnetic iron oxide, is characterized in that, comprises the following steps:
(1) respectively molysite and anion surfactant are dissolved in deionized water, stir and obtain clear solution, then by two kinds of solution hybrid reactions, magnetic agitation;
(2) by the reaction solution centrifugation that step (1) obtains, remove supernatant liquor, washing, drying, obtain grain of rice shape iron carbonyl oxide compound;
(3) grain of rice shape iron carbonyl oxide compound step (2) obtained is heat-treated in the certain atmosphere of certain temperature, namely obtains rice-granule nano magnetic iron oxide.
2. the preparation method of rice-granule nano magnetic iron oxide according to claim 1, is characterized in that, in described step (1), molysite is the one in FERRIC CHLORIDE ANHYDROUS, Iron(III) chloride hexahydrate, ferric sulfate, iron nitrate.
3. the preparation method of rice-granule nano magnetic iron oxide according to claim 1, it is characterized in that, in described step (1), anion surfactant is the one in cetyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, Trimethyllaurylammonium bromide, Sodium dodecylbenzene sulfonate.
4. the preparation method of rice-granule nano magnetic iron oxide according to claim 1, is characterized in that, in described step (1), the mol ratio of anion surfactant and molysite is 0 ~ 2.
5. the preparation method of rice-granule nano magnetic iron oxide according to claim 1, is characterized in that, in described step (1), the hybrid reaction time is 40-100 DEG C, and the reaction times is 2-12h.
6. the preparation method of rice-granule nano magnetic iron oxide according to claim 1, is characterized in that, in described step (3), heat treated temperature is 200-450 DEG C, and heat treatment time is 1-4h, and heat treated atmosphere is vacuum or hydrogen.
7. the preparation method of rice-granule nano magnetic iron oxide according to claim 1, is characterized in that, washing step is in described step (2): first with deionized water by product cleaning 3 times, then use absolute ethanol washing, centrifugal; Described drying is 50 DEG C of dried overnight.
8. the application of rice-granule nano magnetic iron oxide in surface reinforced Raman active base material obtained by preparation method described in any one of claim 1-7.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110104692A (en) * | 2019-05-16 | 2019-08-09 | 南京航空航天大学 | One kind having anisotropic magnetic iron ore electromagnetic-wave absorbent and preparation method thereof |
| CN112320852A (en) * | 2020-11-23 | 2021-02-05 | 湖北大学 | Preparation method of spindle-shaped nano iron oxyhydroxide |
| WO2023201973A1 (en) * | 2022-04-22 | 2023-10-26 | 浙江华源颜料股份有限公司 | Synthesis method for wide-chromatographic-band iron oxide yellow pigment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1427042A (en) * | 2001-12-17 | 2003-07-02 | 暨南大学 | Manufacturing method of nano iron oxide powder |
| CN101117241A (en) * | 2007-07-16 | 2008-02-06 | 中国科学院上海硅酸盐研究所 | Ferrum oxidate nano magnetic material and method for preparing the same |
| CN103043726A (en) * | 2012-12-03 | 2013-04-17 | 云南云天化股份有限公司 | Preparation method of ellipsoidal particle size-controllable alpha-Fe2O3 nano particle |
| CN104150541A (en) * | 2014-09-03 | 2014-11-19 | 安徽工业大学 | Preparation method for rice grain-shaped alpha-Fe2O3 (alpha-ferric oxide) nanometer powder |
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2015
- 2015-08-09 CN CN201510480659.6A patent/CN105129862B/en not_active Expired - Fee Related
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| CN1427042A (en) * | 2001-12-17 | 2003-07-02 | 暨南大学 | Manufacturing method of nano iron oxide powder |
| CN101117241A (en) * | 2007-07-16 | 2008-02-06 | 中国科学院上海硅酸盐研究所 | Ferrum oxidate nano magnetic material and method for preparing the same |
| CN103043726A (en) * | 2012-12-03 | 2013-04-17 | 云南云天化股份有限公司 | Preparation method of ellipsoidal particle size-controllable alpha-Fe2O3 nano particle |
| CN104150541A (en) * | 2014-09-03 | 2014-11-19 | 安徽工业大学 | Preparation method for rice grain-shaped alpha-Fe2O3 (alpha-ferric oxide) nanometer powder |
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| 张霞等: ""纺锤形β-FeOOH的形成过程研究"", 《化学物理学报》 * |
| 杜晶晶等: ""Fe3O4@Ag表面增强拉曼活性基底的制备及其对水中持久性有机污染物的富集和监测"", 《中国化学会第二十七届学术年会》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110104692A (en) * | 2019-05-16 | 2019-08-09 | 南京航空航天大学 | One kind having anisotropic magnetic iron ore electromagnetic-wave absorbent and preparation method thereof |
| CN112320852A (en) * | 2020-11-23 | 2021-02-05 | 湖北大学 | Preparation method of spindle-shaped nano iron oxyhydroxide |
| WO2023201973A1 (en) * | 2022-04-22 | 2023-10-26 | 浙江华源颜料股份有限公司 | Synthesis method for wide-chromatographic-band iron oxide yellow pigment |
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