CN101694799B - Preparation method of trimanganese tetroxide nanoparticles with magneto-optical double functions - Google Patents
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Abstract
The invention relates to a preparation method of trimanganese tetroxide nanoparticles with magneto-optical double functions, which belongs to a preparation method of nanoparticles with magneto-optical double functions. The magneto-optical double functional nanoparticles prepared in the prior art has the defects of unstable optical property and easy quenching of fluorescence of luminants. The preparation method comprises the following steps: preparing a manganese acetylacetonate precursor; preparing oil soluble trimanganese tetroxide nanoparticles with surfaces having oleyl amine for coordination; preparing cyclohexane solution; preparing water soluble trimanganese tetroxide nanoparticles coated by silicon dioxide, wherein the surfaces of the water soluble trimanganese tetroxide nanoparticles have a great deal of amino groups; and preparing water soluble trimanganese tetroxide nanoparticles with the magneto-optical double functions. The invention has the advantages that the nanoparticles have stable magnetism, good luminous performance and difficultly quenched fluorescence; the preparation device is simple; the prepared particles have uniform grain diameter, good dispersity and good water solubility; the raw materials are easily obtained and have low cost; the operation is simple; and no pollution to the environment is generated.
Description
Technical field
The invention belongs to the preparation method of magneto-optic dual-function nanoparticle, specifically a kind of preparation method with magneto-optic double-function trimanganese tetroxide nano particle.
Background technology
Magnetic material and luminescent material are historical long, broad-spectrum two kinds of functional materials, the development of it and modern science and technology, and the every field of informationization, automation, electromechanical integration, national defence and national economy is closely related.Magnetic material is meant the material that can directly or indirectly be produced magnetic by elemental iron, cobalt, nickel, manganese and alloy thereof etc.Magnetic material is divided into " metal and alloy magnetic material " and " ferrite magnetic material " two big types; Ferrite magnetic material is divided into two types of polycrystalline structure and mono-crystalline structures materials again.Say that from application function magnetic material is divided into: soft magnetic material, permanent magnetic material, magnetic recording-rectangular hysteresis material, gyromagnetic material multiclass.Luminescent material is claimed luminous element again, be a kind of can be the various forms of power conversion that absorb from the external world functional material of non-equilibrium light radiation.The illumination mode of luminescent material has multiple, and main type has: luminescence generated by light, cathode-ray luminescence, electroluminescence, thermoluminescence, light are released luminous, radioluminescence etc.
Along with the needs of progress of science and technology, people's lives and the development of nanometer technology, people have been deep into more and more littler range scale to the research of nano material, and increasing functional character.The magneto-optic double-function nano material integrates magnetic and luminous, in magnetics, fluorescence, biology, medicine and other fields extensive use with its characteristics such as magnetics and luminescent properties, particular structure well; Particularly have extremely important application, become the great research topic of International Technology circle at aspects such as Ultrahigh-Density Data Storage, biomolecule identification, medicine transmission.All there is strict requirement in field such as biochemistry and medical science to physics, chemistry and pharmacological properties such as chemical composition, granule size, magnetic function, light function, crystal structure, surface topography, dissolubility and the toxicity etc. of magneto-optic double-function nano material.Realization has the application of the nano material of magneto-optic double-function in fields such as biochemistry and medical science, must meet the following conditions: have magnetic performance and luminescent properties simultaneously 1.; 2. luminous element fluorescence is not easy quencher; 3. have water-soluble; 4. has monodispersity preferably.
The prior art for preparing water-soluble magnetic nanoparticle, in nanoparticle surface modified main means: organic polymer coats, ligand exchange.Organic polymer coats, and causes particle aggregation easily, and nanoparticle dissolution property is unstable.Ligand exchange method time efficiency is low, and the preparation process is complicated.After adopting the magnetic nano-particle of above-mentioned prior art for preparing to connect luminescent material, significant disadvantages is the fluorescent ligand fluorescent quenching that causes the surface to connect easily, thus the difficult purpose that realizes magneto-optic double-function.The shortcoming of the magneto-optic dual-function nanoparticle of prior art for preparing is: 1. have magnetic property, optical property is unstable; 2. the easy quencher of luminous element fluorescence.Because the magneto-optic dual-function nanoparticle of preparation has above-mentioned shortcoming, can't satisfy the application conditions in fields such as biochemistry and medical science, has limited the application of magneto-optic dual-function nanoparticle.Therefore it is crucial inventing a kind of new method for preparing magneto-optic dual-function nanoparticle.
The present invention connects luminous organic material at particle surface then through the silicon dioxide coated nano particle.Make nano particle have magnetics, luminous difunctional, have good dispersiveness and water-soluble simultaneously.The characteristics of this structure are that surperficial luminous organic material is relatively large with the nanoparticle core distance with magnetic, and luminescent material can not cause fluorescent quenching because of the effect of magnetic influence of magnetic nano particle daughter nucleus.Synthetic method of the present invention is simple, advantages such as reaction condition is gentle, required raw material are easy to get, cheap, operating process convenience, non-environmental-pollution.Use simple reaction unit can prepare the trimanganese tetroxide nano particle with magneto-optic double-function of uniform particle diameter, good dispersion, good water solubility.
Through extensively retrieving domestic and international patent document and public publication, all not seeing has the method that prepare magneto-optic dual-function nanoparticle identical with the present invention.The present invention has novelty, creativeness, practicality.
Summary of the invention:
The purpose of this invention is to provide a kind of preparation method with magneto-optic double-function trimanganese tetroxide nano particle.
The objective of the invention is to realize like this:
The preparation method of magneto-optic double-function trimanganese tetroxide nano particle comprises the steps:
The preparation manganese acetylacetonate precursor: getting 1.96 weight portion concentration is 10 mM MnCl
24H
2O is dissolved in 10 weight parts waters; In above-mentioned solution, adding 4 weight portion concentration is 40 mM acetylacetone,2,4-pentanediones; Stirred 15 minutes under the room temperature; Add 3 weight portion triethylamines; Yellow mercury oxide in the abstraction reaction liquid also filters;
The dose volume ratio is 8: 2 ethanol and a water mixed solution, the yellow solid that obtains is filtered in extraction be added in ethanol, the water mixed solution, keeps 70 ℃ of temperature, is stirred to dissolving fully; The room temperature cooling, yellow acicular crystal in the filtering solution gets manganese acetylacetonate precursor;
(2) the surperficial oleyl amine coordination oil-soluble trimanganese tetroxide nano particle of preparation: get the 0.3 weight portion manganese acetylacetonate precursor that above-mentioned steps makes and be dissolved in the 7.61 weight portion oleyl amines; Vacuumize; Magnetic agitation in nitrogen atmosphere is heated rapidly to 170 ℃, isothermal reaction 12 hours; Centrifugalize after being cooled to room temperature; Material after the separation is washed 5 times with absolute ethyl alcohol continuously; Vacuumize; Make the brown material oil-soluble trimanganese tetroxide nano particle of surperficial oleyl amine coordination;
(3) compound concentration is 60 milligrams every milliliter a cyclohexane solution; With 6.0 mM α-(4-nonyl phenyl)-ω-hydroxyl-gather (oxidation-1,2-joins ethane) surfactant (Igepal CO-520), add in the cyclohexane solution ultrasonic dissolution;
(4) get the oil-soluble trimanganese tetroxide nano particle vacuumize of step (2) preparation, add in the solution that step (3) makes, be mixed with concentration and be 55 milligrams every milliliter cyclohexane solution;
(5) two kinds of solution that step (3), (4) made mix, and ultrasonic dissolution is even, inserts in the container, add concentrated ammonia liquor, positive tetraethyl orthosilicate, 3-aminopropyl-triethoxysilane successively, and stirring at normal temperature 8-12 hour, centrifugation; Respectively wash 4 times with the second alcohol and water respectively, there is the water-soluble trimanganese tetroxide nano particle of a large amount of amino on the surface that makes coated with silica;
(6) preparation has the water-soluble trimanganese tetroxide nano particle of magneto-optic double-function:
Get the water-soluble trimanganese tetroxide nano particle of the coated with silica of step (5) preparation, be dissolved in the oxolane that anhydrates; Add rhodamine isothiocyanate; Sealing vacuumizes, nitrogen protection; The masking foil lucifuge; Stirring at room 10 hours; Centrifugation with absolute ethanol washing 5 times, makes the water-soluble trimanganese tetroxide nano particle that coated with silica has magneto-optic double-function.
Step (5) adds concentrated ammonia liquor, positive tetraethyl orthosilicate, 3-aminopropyl-triethoxysilane (after adding concentrated ammonia liquor, the pH value of mixed solution is adjusted to 7.5-8.0) successively.
Rhodamine isothiocyanate excitation spectrum 488 nanometers in the step (6), emission spectrum 550-600 nanometer, send yellow orange light.
The water-soluble trimanganese tetroxide nano particle diameter 30-38 nanometer that step (6) makes with magneto-optic double-function.
The present invention at first prepares oil-soluble magnetic nano-particle through the method for thermal decomposition; Then with this nanoparticle surface coated silica; Not only nano particle has water-soluble while surface and has a large amount of amino; Be connected to nanoparticle surface through rhodamine isothiocyanate (RBITC) and amino effect then; Make nano particle also have good luminescent properties, add the trimanganese tetroxide nano particle and itself have magnetic property preferably, thereby realize synthetic purpose with water-soluble manganic manganous oxide nano-material of magneto-optic double-function.
Main points of the present invention are: utilize coated with silica and be connected luminous organic material preparation and have magnetics, luminous bifunctional water-soluble manganic manganous oxide nano-material.This material has nucleocapsid structure, is that nuclear, silicon dioxide are shell with magnetic trimanganese tetroxide nano particle, the organic dyestuff that the finishing of shell is luminous.Uniform particle diameter, good dispersion, good water solubility, have good magnetic property and luminescent properties, bio-compatibility is good.Make through following method: be solvent and surfactant with the oleyl amine; Thermal decomposition presoma manganese acetylacetonate in air atmosphere; Obtain the mangano-manganic oxide magnetic nano-particle; Vacuumize is dissolved in dried trimanganese tetroxide nano particle in the cyclohexane solution of every milliliter of 50-60 milligram then.Add the positive tetraethyl orthosilicate of 180-200 microlitre (TEOS), 50-60 microlitre 3-aminopropyl-triethoxysilane (APS) again, 2.5-3.0 gram surfactant is dissolved in the cyclohexane solvent; At pH is 7.5-8.0 weak basic condition stirring at room 20-24 hour; Obtain the water-soluble trimanganese tetroxide nano particle of particle diameter 28-36 nanometer amino functional; Then nano particle and organic dyestuff are dissolved in the 80-100 milliliter anhydrous tetrahydro furan; Stirred 8-10 hour, centrifugation, thus obtain the water-soluble trimanganese tetroxide nano particle that the 30-38 nanometer has magneto-optic double-function.Organic dyestuff be excitation spectrum 488 nanometers, emission spectrum in the 550-600 nanometer, send yellow orange light.
Essential implementation of the present invention is: utilize oleyl amine as solvent and surfactant, and thermal decomposition manganese acetylacetonate precursor in air, obtaining surface ligand is the oil-soluble mangano-manganic oxide magnetic nano-particle of oleyl amine; When the present invention prepares oil-soluble trimanganese tetroxide nano nuclear, can be in nitrogen atmosphere, also can be in air atmosphere the pyrolysis precursor; Finally obtain trimanganese tetroxide nano particle with a kind of crystal formation.First step temperature range in the heating pyrolysis is 85-95 ℃, and in this temperature range, it is state of atom that presoma begins by pyrolysis.Be heated to 150-160 ℃, atom begins to re-assembly, nucleation, crystallization, forms the trimanganese tetroxide nano particle.The trimanganese tetroxide nano magnetic particle pattern that the present invention makes is main with sphere, and average diameter is the 6-11 nanometer, and the trimanganese tetroxide nano magnetic particle of preparation shows paramagnetism preferably.Wrap up the silicon dioxide shell on trimanganese tetroxide nano magnetic particle surface then, dexterously oil-soluble nano particle is changed into the water-soluble trimanganese tetroxide nano particle of amino functional; Again through the amino luminous organic material that connects.The nano particle that this method is prepared can well be scattered in the water, and has good magneto-optic double-function and excellent biological compatibility.To equipment require low; The needed raw material price is low; Accessory substance is nuisanceless, environmentally safe.
When the present invention prepares the water-soluble mangano-manganic oxide magnetic Nano material of amino functional; Cyclohexane is a solvent; Oil-soluble trimanganese tetroxide nano particle is made into the cyclohexane solution that concentration is every milliliter of 50-60 milligram; Adding 2.5-3.0 gram α-(4-nonyl phenyl)-ω-hydroxyl-gather (oxidation-1,2-joins ethane) surfactant (Igepal CO-520), mixed solution is ultrasonic evenly; With concentrated ammonia liquor mixed solution is regulated the weakly alkaline solution that becomes pH=7.5-8.0, added the positive tetraethyl orthosilicate of 180-200 microlitre (TEOS) and 50-6 microlitre 3-aminopropyl-triethoxysilane (APS) again stirring at normal temperature 20-24 hour; Centrifugation; Promptly obtain the magnetic Nano material that the surface has amino mangano-manganic oxide/silicon dixoide nucleocapsid structure.This material can well be scattered in the aqueous solution, and the amino through the luminous organic material nanoparticle surface connects again, makes it have good luminescent properties, finally can realize the magneto-optic double-function of water-soluble trimanganese tetroxide nano particle.
The present invention is because the surface of silicon dioxide has more amino, so can connect more luminescent material; Because luminescent material is far away apart from magnetic Nano nuclear, so fluorescence is difficult for quencher, has guaranteed the stability of luminescent properties.
Advantage of the present invention is:
1. the magneto-optic double-function trimanganese tetroxide nano particle magnetic stability that makes, good luminous performance, fluorescence is difficult for quencher.
2. preparation facilities is simple;
The particle diameter of preparation evenly, good dispersion, good water solubility;
Raw material be easy to get, cheap;
5. simple to operate; Environmentally safe.
6. magneto-optic double-function trimanganese tetroxide nano particle is widely used at medicine and biological field.
Description of drawings:
Fig. 1 is that surface organic ligands that the present invention synthesizes is the X ray diffracting spectrum (XRD figure) that there is the trimanganese tetroxide nano particle of a large amount of amino on the surface behind X ray diffracting spectrum (XRD figure) and the coated silica shell of trimanganese tetroxide nano particle of oleyl amine.Fig. 1 shows that the trimanganese tetroxide nano particle that makes is hausmannite type (the card sequence number 24-0734 of JCPDS).
Fig. 2 is that the surface organic ligands that the present invention synthesizes is the transmission electron microscope collection of illustrative plates (TEM figure) of the trimanganese tetroxide nano particle of oleyl amine.Fig. 2 shows that the trimanganese tetroxide nano particle has monodispersity preferably in n-hexane, and particle diameter is the even circle of 6-11 nanometer.
Fig. 3 is the transmission electron microscope collection of illustrative plates (TEM figure) that there is the trimanganese tetroxide nano particle of a large amount of amino on the surface behind the coated silica shell that synthesizes of the present invention; Fig. 3 is illustrated in has good monodispersity in the aqueous solution, only contain a trimanganese tetroxide nano nuclear in each particle.
Fig. 4 is the infrared ray collection of illustrative plates (IR figure) of the forward and backward trimanganese tetroxide nano particle of the coated silica shell that synthesizes of the present invention; Surface before the parcel is the trimanganese tetroxide nano particle of oleyl amine, 422.3cm
-1, 516.8cm
-1, 422.3cm
-1Be the characteristic peak that the manganese oxygen key stretching vibration of mangano-manganic oxide particle produces, 1120.3cm
-1Be the oleyl amine C-N stretching vibration of nanoparticle surface, 1633.6cm
-1Be the stretching vibration of the oleyl amine C=C of nanoparticle surface, 2925.5cm
-1Stretching vibration for the oleyl amine C-H of nanoparticle surface; After the coated silica, can obviously see 1056.8cm
-1Be Si-O-Si asymmetric stretching vibration, 452.4cm
-1, 782.4cm
-1, 957.4cm
-1δ for silicon dioxide
Si-OThe deformation vibration characteristic peak, 1561.3cm
-1Flexural vibrations 1639.5cm for the oleyl amine N-H of nanoparticle surface
-1Be the stretching vibration of the oleyl amine C=C of nanoparticle surface, owing to added APS during reaction, so the trimanganese tetroxide nano particle surface of coated with silica has amino, 3426.6cm
-1Possibly be-NH
2Flexural vibrations.
Fig. 5 is the water-soluble photo of the trimanganese tetroxide nano particle of (1) back (2) before the coated silica shell that synthesizes of the present invention.
Fig. 6 is the uv absorption figure before and after mangano-manganic oxide/silica core-shell nanostructured surface connects the rhodamine isothiocyanate luminous element that the present invention synthesizes.
Fig. 7 is the fluorescence spectrum figure after mangano-manganic oxide/silica core-shell nanostructured surface connects the rhodamine isothiocyanate luminous element that the present invention synthesizes.
Fig. 8 be the present invention synthesize connect rhodamine isothiocyanate luminous element (1) and excite the photo of (2) down under white light at mangano-manganic oxide/silica core-shell nanostructured surface at 254 nanometer uviol lamps.Fig. 8 is illustrated in 254 nanometer uviol lamps and excites down and send bright yellow orange light.
Embodiment:
Through embodiment the present invention is further specified below, but content of the present invention is not limited thereto.
Embodiment 1:
The preparation manganese acetylacetonate precursor.
Take by weighing MnCl
24H
2O (1.979 grams, 10 mMs) is dissolved in 10 ml waters; In above-mentioned solution, add 4.1 milliliters then, 40 mM acetylacetone,2,4-pentanediones; Room temperature condition stirred 15 minutes down; In solution, add 3 milliliters of triethylamines again, occur yellow mercury oxide in the reactant liquor, extract filtering precipitate.
The dose volume ratio is 8: 2 20 milliliters of ethanol and a water mixed solution, filters the yellow solid that obtains and is added in ethanol, the water mixed solution extracting, and under 70 ℃ of temperature, is stirred to dissolving fully; Room temperature cooling then produces yellow acicular crystal in the solution, filter; Get yellow acicular crystal manganese acetylacetonate precursor.
Embodiment 2:
Prepare surperficial oleyl amine coordination oil-soluble trimanganese tetroxide nano particle.
Get manganese acetylacetonate precursor 0.30 gram that instance 1 makes, 1.19 mMs are dissolved in 7.61 grams; 28.44 in the mM oleyl amine, it is inserted 100 milliliters of three-neck flasks, vacuumizes; Magnetic agitation in nitrogen atmosphere is heated rapidly to 170 ℃, isothermal reaction 12 hours; Centrifugalize after being cooled to room temperature; Material after the separation is washed 5 times with absolute ethyl alcohol continuously; Vacuumize; Get brown material, be surperficial oleyl amine coordination oil-soluble trimanganese tetroxide nano particle.
Embodiment 3:
There is the water-soluble trimanganese tetroxide nano particle of a large amount of amino on the surface of preparation coated with silica.
Take by weighing surfactant 6.0 mM α-(4-nonyl phenyl)-ω-hydroxyl-gather (oxidation-1,2-joins ethane) surfactant (Igepal CO-520) 2.8 grams, put into 50 ml beakers, add 30 milliliters of cyclohexanes, ultrasonic dissolution.It is 55 milligrams every milliliter cyclohexane solution that the oil-soluble trimanganese tetroxide nano particle of getting embodiment 2 preparation is configured to 150 microlitre concentration.Two kinds of solution are mixed, and ultrasonic dissolution is even, inserts in 250 milliliters the conical flask; The concentrated ammonia liquor that adds 200 microlitres successively, the positive tetraethyl orthosilicate of 190 microlitres (TEOS), 55 microlitre 3-aminopropyl-triethoxysilanes (APS); Stirring at normal temperature 12 hours; Centrifugation is washed respectively 4 times with ethanol and water, and there is the water-soluble trimanganese tetroxide nano particle of a large amount of amino on the surface that promptly obtains coated with silica.
Embodiment 4:
Get 30 milligrams on the water-soluble trimanganese tetroxide nano particle of the coated with silica of embodiment 3 preparation, be dissolved in 80 milliliters of oxolanes that anhydrate, insert 100 milliliters of round-bottomed flasks; The rhodamine isothiocyanate that adds 2.5 milligrams; Sealing vacuumizes, nitrogen protection; The masking foil lucifuge; Stirring at room 10 hours.Centrifugation with absolute ethanol washing 5 times, makes the water-soluble trimanganese tetroxide nano particle with magneto-optic double-function of coated with silica.
The foregoing description is merely preference of the present invention, is not used for limiting the present invention, and is all within principle of the present invention, and any modification and the variation made are all within protection scope of the present invention.
Claims (4)
1. the preparation method of a magneto-optic double-function trimanganese tetroxide nano particle comprises the steps:
(1) preparation manganese acetylacetonate precursor: get 10 mM MnCl
24H
2O is dissolved in 10 ml waters; In above-mentioned solution, add 40 mM acetylacetone,2,4-pentanediones; Stirred 15 minutes under the room temperature; Add 3 milliliters of triethylamines; Yellow mercury oxide in the abstraction reaction liquid also filters;
The dose volume ratio is 8: 2 ethanol and a water mixed solution, the yellow solid that obtains is filtered in extraction be added in ethanol, the water mixed solution, keeps 70 ℃ of temperature, is stirred to dissolving fully; The room temperature cooling, yellow acicular crystal in the filtering solution gets manganese acetylacetonate precursor;
(2) the surperficial oleyl amine coordination oil-soluble trimanganese tetroxide nano particle of preparation: get the 0.3 weight portion manganese acetylacetonate precursor that above-mentioned steps makes and be dissolved in the 7.61 weight portion oleyl amines; Vacuumize; Magnetic agitation in nitrogen atmosphere is heated rapidly to 170 ℃, isothermal reaction 12 hours; Centrifugalize after being cooled to room temperature; Material after the separation is washed 5 times with absolute ethyl alcohol continuously; Vacuumize; Make the brown material oil-soluble trimanganese tetroxide nano particle of surperficial oleyl amine coordination;
(3) compound concentration is the cyclohexane solution of every milliliter of 0.5 mM: with 6.0 mM α-(4-nonyl phenyl)-ω-hydroxyl-gather (oxidation-1,2-joins ethane) surfactant, add in the cyclohexane solution ultrasonic dissolution;
(4) get the oil-soluble trimanganese tetroxide nano particle of step (2) preparation, add in the solution that step (3) makes, be mixed with concentration and be 55 milligrams every milliliter cyclohexane solution;
(5) two kinds of solution that step (3), (4) made mix, and ultrasonic dissolution is even, inserts in the container, add concentrated ammonia liquor, positive tetraethyl orthosilicate, 3-aminopropyl-triethoxysilane successively, and stirring at normal temperature 8-12 hour, centrifugation; Respectively wash 4 times with the second alcohol and water respectively, there is the water-soluble trimanganese tetroxide nano particle of a large amount of amino on the surface that makes coated with silica;
(6) preparation has the water-soluble trimanganese tetroxide nano particle of magneto-optic double-function:
Get the water-soluble trimanganese tetroxide nano particle of the coated with silica of step (5) preparation, be dissolved in the anhydrous tetrahydro furan; Add rhodamine isothiocyanate; Sealing vacuumizes, nitrogen protection; The masking foil lucifuge; Stirring at room 10 hours; Centrifugation with absolute ethanol washing 5 times, makes the water-soluble trimanganese tetroxide nano particle with magneto-optic double-function of coated with silica.
2. the preparation method of magneto-optic double-function trimanganese tetroxide nano particle according to claim 1 is characterized in that: step (5) adds concentrated ammonia liquor, positive tetraethyl orthosilicate, 3-aminopropyl-triethoxysilane successively; After adding concentrated ammonia liquor, the pH value of mixed solution is adjusted to 7.5-8.0.
3. the preparation method of magneto-optic double-function trimanganese tetroxide nano particle according to claim 1 is characterized in that: rhodamine isothiocyanate excitation spectrum 488 nanometers in the step (6), emission spectrum 550-600 nanometer, send yellow orange light.
4. the preparation method of magneto-optic double-function trimanganese tetroxide nano particle according to claim 1 is characterized in that: the water-soluble trimanganese tetroxide nano particle diameter 30-38 nanometer with magneto-optic double-function that step (6) makes.
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| 何秋星等.纳米磁性Mn3O4粉末的溶剂热法合成及表征.《磁性材料及器件》.2004,第35卷(第4期), * |
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