CN104261488B - A kind of nanometer Fe3O4The preparation method of octahedral structure - Google Patents
A kind of nanometer Fe3O4The preparation method of octahedral structure Download PDFInfo
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- CN104261488B CN104261488B CN201410506710.1A CN201410506710A CN104261488B CN 104261488 B CN104261488 B CN 104261488B CN 201410506710 A CN201410506710 A CN 201410506710A CN 104261488 B CN104261488 B CN 104261488B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- HOIQWTMREPWSJY-GNOQXXQHSA-K iron(3+);(z)-octadec-9-enoate Chemical compound [Fe+3].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O HOIQWTMREPWSJY-GNOQXXQHSA-K 0.000 claims abstract description 35
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 23
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 18
- -1 octadecylene Chemical group 0.000 claims abstract description 18
- 239000000376 reactant Substances 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 12
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 12
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 12
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000005642 Oleic acid Substances 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 12
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 32
- 239000008187 granular material Substances 0.000 abstract description 27
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000011261 inert gas Substances 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 description 10
- 238000001816 cooling Methods 0.000 description 10
- 238000003786 synthesis reaction Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000003704 aspartic acid Nutrition 0.000 description 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011554 ferrofluid Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of nanometer Fe3O4The preparation method of octahedral structure, comprises the following steps: by iron oleate, oleyl amine and octadecylene mix homogeneously, react under inert gas shielding; Centrifugal reaction solution after reaction, by gained washing of precipitate, is nanometer Fe3O4Octahedral structure. Gained nanometer Fe3O4The particle size of octahedral structure is 13-20nm. Preparation technology of the present invention is simple, yield is higher, by accurately controlling the parameters such as the ratio of reactant, reaction temperature, response time, it is possible to obtain the nanometer Fe of good dispersion, narrow size distribution3O4Octahedral structure, to small size nanometer Fe3O4The regulating microstructure of granule and physicochemical characteristic research thereof are significant.
Description
Technical field
The present invention relates to a kind of nanometer Fe3O4The preparation method of granule, is specifically related to the nanometer Fe of a kind of size adjustable3O4The preparation method of octahedral structure.
Background technology
Magnetic nanoparticle is a class nano structural material widely studied at present, plays an important role in applications such as medical treatment, advanced technologies. Nanometer Fe3O4Granule is the Typical Representative of magnetic Nano material, has huge application prospect in medicine conveying, magnetic data storage, bio-molecular separation, bio-sensing, ferrofluid etc. Particle size distribution is narrow, the nanometer Fe of size tunable3O4The building-up process of granule is always up the hot issue of research, and Fe3O4Granule is obtained in that unique physicochemical properties at the Morphological control of nanoscale scope, is increasingly subject to the common concern of scholars.
Both at home and abroad about Fe3O4The report of octahedral structure is relatively fewer, and main preparation methods has hydro-thermal method, seed assisting growth method etc. Document " XiaofeiQu; GentaoZhou; QizhiYao; andShengquanFu.J.Phys.Chem.C; 2010,114,284-289 " reports with iron chloride for source of iron, aspartic acid is reducing agent, adopts the hydro-thermal method of biomolecule auxiliary to prepare distribution of sizes homogeneous micron order (1-5 μm) Fe3O4The method of octahedra granule; Document " DongenZhang; XiaojunZhang; XiaominNi; JimeiSong, andHuaguiZheng.CrystalGrowth&Design, 2007; 7 (10); 2117-2119 " reports with iron chloride for source of iron, and hydrazine hydrate is reducing agent, adopts the Fe that the hydro-thermal method preparation that ethylenediaminetetraacetic acid (EDTA) is assisted is of a size of 0.2-1.6 μm3O4The method of octahedra granule; Document " QingSong, YongDing, ZhonglinWang, andZ.JohnZhang.J.Phys.Chem.B, 2006,110,25547-25550 " reports with spherical Fe3O4Nanocrystalline for seed, ferric acetyl acetonade is source of iron, is incubated 2h preparation at 220 DEG C and is uniformly dispersed, is of a size of the Fe of about 10nm3O4The method of octahedra granule.
Currently for nanometer Fe3O4The research of octahedral structure is deep not enough, preparation process relative complex, relatively costly, is unfavorable for accurately controlling and industrialized production.
Summary of the invention
The present invention is directed to the deficiency that existing method exists, it is provided that a kind of nanometer Fe3O4The preparation method of octahedral structure, the method is simple to operate, and yield is high, gained nanometer Fe3O4Octahedral structure narrow size distribution, size adjustable, good dispersion.
The concrete technical scheme of the present invention is as follows:
A kind of nanometer Fe3O4The preparation method of octahedral structure, comprises the following steps:
(1) by iron oleate, oleyl amine and octadecylene (ODE) mix homogeneously, react under protective gas is protected;
(2) centrifugal reaction solution after reaction, by gained washing of precipitate, is nanometer Fe3O4Octahedral structure.
In above-mentioned steps (1), the volume ratio of iron oleate and oleyl amine is 1:1.2-2.
In above-mentioned steps (1), the volume ratio of iron oleate and octadecylene is 1:5-7.
In above-mentioned steps (1), reaction temperature is 310-320 DEG C.
In above-mentioned steps (1), the response time is 15-60min.
In above-mentioned steps (1), described protective gas is preferably nitrogen.
In above-mentioned preparation method, iron oleate used can adopt any iron oleate preparation method disclosed in prior art to prepare. In the embodiment of the present invention, iron oleate adopts following methods to prepare: is mixed homogeneously with dehydrated alcohol by oleic acid, joins in ferric chloride in aqueous solution, at room temperature stirs to reacting completely; Reacting addition normal hexane in backward reactant liquor, separatory after standing, gained iron oleate is standby after drying.
The present invention can be relatively simple obtain nanometer Fe3O4Octahedral structure, gained nanometer Fe3O4Octahedral structure is of a size of 13-20nm, and dimensional controllability is strong.
The present invention is simply and efficiently prepared for the nanometer Fe that good dispersion, narrow size distribution, size are controlled3O4Octahedral structure, by parameters such as Precise Control of Oil acid ferrum, oleyl amine and the volume ratio of octadecylene, reaction temperature, response time, it is possible to obtain the nanometer Fe of size and morphology controllable3O4Octahedra granule. When other experiment conditions remain unchanged, the volume ratio of iron oleate, oleyl amine and octadecylene is regulation and control nanometer Fe3O4One of key factor of octahedral structure. When the volume ratio of iron oleate, oleyl amine and octadecylene is 1:1.2-2:5-7, it is possible to obtain nanometer Fe3O4Octahedral structure. By changing reaction temperature and response time, it is possible to regulation and control nanometer Fe3O4The size of octahedra granule.
The invention provides one and accurately prepare nanometer Fe3O4The method of octahedral structure, gained nanometer Fe3O4The particle size of octahedral structure is 13-20nm. Preparation technology of the present invention is simple, yield is higher, by accurately controlling the parameters such as the ratio of reactant, reaction temperature, response time, it is possible to obtain the nanometer Fe of good dispersion, narrow size distribution3O4Octahedral structure, to small size nanometer Fe3O4The regulating microstructure of granule and physicochemical characteristic research thereof are significant.
Accompanying drawing explanation
Fig. 1 is the Fe of the embodiment of the present invention 1 synthesis3O4Transmission electron microscope (TEM) picture of octahedra granule.
Fig. 2 is the Fe of the embodiment of the present invention 1 synthesis3O4X-ray diffraction (XRD) collection of illustrative plates of octahedra granule.
Fig. 3 is the Fe of the embodiment of the present invention 1 synthesis3O4Hysteresis curve (VSM) collection of illustrative plates of octahedra granule.
Fig. 4 is the Fe of the embodiment of the present invention 3 synthesis3O4Transmission electron microscope (TEM) picture of octahedra granule.
The Fe of Fig. 5 embodiment of the present invention 6 synthesis3O4Transmission electron microscope (TEM) picture of octahedra granule.
The Fe of Fig. 6 embodiment of the present invention 8 synthesis3O4Transmission electron microscope (TEM) picture of octahedra granule.
The Fe of Fig. 7 comparative example 1 synthesis of the present invention3O4Transmission electron microscope (TEM) picture of irregular particle.
Detailed description of the invention
The present invention will be further elaborated by the examples below, and its content, only for explaining the present invention, is not defined by the description below.
Embodiment 1
1.1, by 8.86mL oleic acid and 32mL dehydrated alcohol mix homogeneously, join in 25mL ferric chloride in aqueous solution (c=0.371mol/L), at room temperature stir to reacting completely;
1.2 add 15mL normal hexane in above-mentioned reactant liquor, after pyriform funnel separatory, are placed in the baking oven of 110 DEG C and are incubated 5h obtain iron oleate;
5mL iron oleate, 8mL oleyl amine and 30mL octadecylene are placed in four-hole bottle mix homogeneously by 1.3, at N2It is heated to 310 DEG C under protection, is incubated 30min;
1.4, by the sample centrifugation after cooling, washing, obtain being of a size of the Fe of 14nm3O4Octahedra granule, the microscopic appearance of product, phase structure and magnetic property are distinguished as shown in Figure 1,2 and 3, it can be seen that product is uniformly dispersed, soilless sticking.
Embodiment 2
2.1, by 8.86mL oleic acid and 32mL dehydrated alcohol mix homogeneously, join in 25mL ferric chloride in aqueous solution (c=0.371mol/L), at room temperature stir to reacting completely;
2.2 add 15mL normal hexane in above-mentioned reactant liquor, after pyriform funnel separatory, are placed in the baking oven of 110 DEG C and are incubated 5h obtain iron oleate;
5mL iron oleate, 6mL oleyl amine and 25mL octadecylene are placed in four-hole bottle mix homogeneously by 2.3, at N2It is heated to 310 DEG C under protection, is incubated 60min;
2.4, by the sample centrifugation after cooling, washing, obtain being of a size of the Fe of 17.5nm3O4Octahedra granule.
Embodiment 3
3.1, by 8.86mL oleic acid and 32mL dehydrated alcohol mix homogeneously, join in 25mL ferric chloride in aqueous solution (c=0.371mol/L), at room temperature stir to reacting completely;
3.2 add 15mL normal hexane in above-mentioned reactant liquor, after pyriform funnel separatory, are placed in the baking oven of 110 DEG C and are incubated 5h obtain iron oleate;
5mL iron oleate, 8mL oleyl amine and 30mL octadecylene are placed in four-hole bottle mix homogeneously by 3.3, at N2It is heated to 310 DEG C under protection, is incubated 20min;
3.4, by the sample centrifugation after cooling, washing, obtain being of a size of the Fe of 13.5nm3O4Octahedra granule, as shown in Figure 4.
Embodiment 4
4.1, by 8.86mL oleic acid and 32mL dehydrated alcohol mix homogeneously, join in 25mL ferric chloride in aqueous solution (c=0.371mol/L), at room temperature stir to reacting completely;
4.2 add 15mL normal hexane in above-mentioned reactant liquor, after pyriform funnel separatory, are placed in the baking oven of 110 DEG C and are incubated 5h obtain iron oleate;
5mL iron oleate, 10mL oleyl amine and 35mL octadecylene are placed in four-hole bottle mix homogeneously by 4.3, at N2It is heated to 310 DEG C under protection, is incubated 50min;
4.4, by the sample centrifugation after cooling, washing, obtain being of a size of the Fe of 16nm3O4Octahedra granule.
Embodiment 5
5.1, by 8.86mL oleic acid and 32mL dehydrated alcohol mix homogeneously, join in 25mL ferric chloride in aqueous solution (c=0.371mol/L), at room temperature stir to reacting completely;
5.2 add 15mL normal hexane in above-mentioned reactant liquor, after pyriform funnel separatory, are placed in the baking oven of 110 DEG C and are incubated 5h obtain iron oleate;
5mL iron oleate, 7mL oleyl amine and 27mL octadecylene are placed in four-hole bottle mix homogeneously by 5.3, at N2It is heated to 320 DEG C under protection, is incubated 25min;
5.4, by the sample centrifugation after cooling, washing, obtain being of a size of the Fe of 14.5nm3O4Octahedra granule.
Embodiment 6
6.1, by 8.86mL oleic acid and 32mL dehydrated alcohol mix homogeneously, join in 25mL ferric chloride in aqueous solution (c=0.371mol/L), at room temperature stir to reacting completely;
6.2 add 15mL normal hexane in above-mentioned reactant liquor, after pyriform funnel separatory, are placed in the baking oven of 110 DEG C and are incubated 5h obtain iron oleate;
5mL iron oleate, 6mL oleyl amine and 30mL octadecylene are placed in four-hole bottle mix homogeneously by 6.3, at N2It is heated to 320 DEG C under protection, is incubated 30min;
6.4, by the sample centrifugation after cooling, washing, obtain being of a size of the Fe of 15nm3O4Octahedra granule, as shown in Figure 5.
Embodiment 7
7.1, by 8.86mL oleic acid and 32mL dehydrated alcohol mix homogeneously, join in 25mL ferric chloride in aqueous solution (c=0.371mol/L), at room temperature stir to reacting completely;
7.2 add 15mL normal hexane in above-mentioned reactant liquor, after pyriform funnel separatory, are placed in the baking oven of 110 DEG C and are incubated 5h obtain iron oleate;
5mL iron oleate, 9mL oleyl amine and 32mL octadecylene are placed in four-hole bottle mix homogeneously by 7.3, at N2It is heated to 320 DEG C under protection, is incubated 55min;
7.4, by the sample centrifugation after cooling, washing, obtain being of a size of the Fe of 19nm3O4Octahedra granule.
Embodiment 8
8.1, by 8.86mL oleic acid and 32mL dehydrated alcohol mix homogeneously, join in 25mL ferric chloride in aqueous solution (c=0.371mol/L), at room temperature stir to reacting completely;
8.2 add 15mL normal hexane in above-mentioned reactant liquor, after pyriform funnel separatory, are placed in the baking oven of 110 DEG C and are incubated 5h obtain iron oleate;
5mL iron oleate, 6mL oleyl amine and 30mL octadecylene are placed in four-hole bottle mix homogeneously by 8.3, at N2It is heated to 320 DEG C under protection, is incubated 40min;
8.4, by the sample centrifugation after cooling, washing, obtain being of a size of the Fe of 18nm3O4Octahedra granule, as shown in Figure 6.
Comparative example 1
1.1, by 8.86mL oleic acid and 32mL dehydrated alcohol mix homogeneously, join in 25mL ferric chloride in aqueous solution (c=0.371mol/L), at room temperature stir to reacting completely;
1.2 add 15mL normal hexane in above-mentioned reactant liquor, after pyriform funnel separatory, are placed in the baking oven of 110 DEG C and are incubated 5h obtain iron oleate;
5mL iron oleate, 8mL oleyl amine and 30mL octadecylene are placed in four-hole bottle mix homogeneously by 1.3, at N2It is heated to 310 DEG C under protection, is incubated 13min;
1.4, by the sample centrifugation after cooling, washing, obtain being of a size of the irregular Fe of pattern of 13nm3O4Granule, as shown in Figure 7.
Comparative example 2
2.1, by 8.86mL oleic acid and 32mL dehydrated alcohol mix homogeneously, join in 25mL ferric chloride in aqueous solution (c=0.371mol/L), at room temperature stir to reacting completely;
2.2 add 15mL normal hexane in above-mentioned reactant liquor, after pyriform funnel separatory, are placed in the baking oven of 110 DEG C and are incubated 5h obtain iron oleate;
5mL iron oleate, 15mL oleyl amine and 30mL octadecylene are placed in four-hole bottle mix homogeneously by 2.3, at N2It is heated to 320 DEG C under protection, is incubated 30min;
2.4, by the sample centrifugation after cooling, washing, obtain being of a size of the spherical Fe of 17nm3O4Granule.
Claims (5)
1. a nanometer Fe3O4The preparation method of octahedral structure, is characterized in that comprising the following steps:
(1) by iron oleate, oleyl amine and octadecylene mix homogeneously, react under protective gas is protected;
(2) centrifugal reaction solution after reaction, by gained washing of precipitate, is nanometer Fe3O4Octahedral structure;
In step (1), the volume ratio of iron oleate and oleyl amine is the volume ratio of 1:1.2-2, iron oleate and octadecylene is 1:5-7;
In step (1), reaction temperature is 310-320 DEG C.
2. preparation method according to claim 1, is characterized in that: in step (1), and the response time is 15-60min.
3. preparation method according to claim 1, is characterized in that: in step (1), and described protective gas is nitrogen.
4. preparation method according to claim 1, is characterized in that: iron oleate adopts following methods to prepare: is mixed homogeneously with dehydrated alcohol by oleic acid, joins in ferric chloride in aqueous solution, at room temperature stirs to reacting completely; Reacting addition normal hexane in backward reactant liquor, separatory after standing, gained iron oleate is standby after drying.
5. preparation method according to claim 1, is characterized in that: gained nanometer Fe3O4Octahedral structure is of a size of 13-20nm.
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CN101525159A (en) * | 2009-04-20 | 2009-09-09 | 中南大学 | Solvothermal preparation method of monodisperse Fe3O4 nano-particles |
CN102153149A (en) * | 2010-12-29 | 2011-08-17 | 济南大学 | Method for preparing nano quantum dot level Fe3O4 superparamagnetic particles |
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