CN104163453B - A kind of preparation method of high-sequential nano particle super crystal lattice material - Google Patents
A kind of preparation method of high-sequential nano particle super crystal lattice material Download PDFInfo
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Abstract
The invention belongs to technical field of inorganic material, be specially a kind of preparation method of high-sequential nano particle super crystal lattice material.The present invention adopts solution method to obtain monodisperse metal oxide nano-crystalline granule, the nanocrystalline superlattice solid of three-dimensional order is prepared by solvent evaporates induced nano particles self assemble, then the organic molecule high temperature cabonization of particle surface is obtained the coated oxide nano particles superlattice of carbon, by acid etch, metal oxide nanoparticles is removed the meso-porous carbon material obtaining high-sequential, take mesoporous carbon as template, in its duct, pour into suitable presoma, the super crystal lattice material of relevant nanometer particle can be obtained finally by means such as hydrolysis, crystallization.The inventive method is simple, and raw material is easy to get, and cost is lower, can be regulated and controled by the particle diameter and pattern controlling starting metals oxide nano-particles to the size of nano particle and pattern.
Description
Technical field
The invention belongs to technical field of inorganic material, be specifically related to a kind of preparation method of high-sequential nano particle super crystal lattice material.
Background technology
Dispersed nano particle is the desirable construction unit constructing Macro-Functions materials and devices, and the super crystal lattice material being formed, have high-sequential by nano-particles self assemble is the class new particulate material risen in recent years, demonstrate important using value in fields such as electronics and opto-electronic device, catalysis, stored energy, information storages.The preparation method of current nano particle super crystal lattice material depends on solvent evaporates induced nano particles self assemble; This method requires that first nano particle will prepare with monodispersed colloidal form, then form superstructure by the slow volatilization induced nano particles self assemble of solvent, therefore the colloidal solution of chemosynthesis dispersed nano particle is the precondition preparing super crystal lattice material.Although a lot of conventional substances, nano particle superlattice as metal, semi-conductor, metal oxide etc. can in this way prepare, but a lot of material, as carbon material, sulfur materials, amorphous oxide, alloy, inorganic salt etc. are difficult to be synthesized with the form of monodisperse colloid nano particle, the preparation of their super crystal lattice materials of therefore also not knowing where to begin.
In nano particle superlattice, each nano particle had both remain self intrinsic particle properties, as quantum effect and dimensional effect etc., simultaneously there is again electron coupling effect between adjacent particle, make superlattice often show collective's synergistic effect not available for single nanoparticle.Interaction between nano particle and the distance between them closely related, therefore, optical, electrical, the magnetic property of nano particle superlattice can be modulated by changing grain spacing in principle.But in fact, the surface of colloidal nanoparticles usually cover by the tensio-active agent ligand molecular (as oleic acid, oleyl amine etc.) of one deck long-chain, insulation, therefore in nano particle superlattice, interaction between adjacent nanoparticles is very faint, limit the embodiment of superlattice collective effect to a great extent, and had a strong impact on electron transport ability, limit its application in catalysis, electronics and opto-electronic device, energy storage field.
The nano particle super crystal lattice material that highly ordered mesosize pores carbon is templated synthesis many kinds of substance is utilized in the present invention, wherein mesoporous carbon obtain by the high temperature cabonization of metal oxide nanoparticles superlattice and acid etch process preparation, and it has three-dimensional continuous, pore passage structure that aperture is adjustable.Product nano particle superlattice not only its particle size can within the scope of 5 ~ 50 nm modulation, and be connected by wicket between adjacent nanoparticles, therefore gained super crystal lattice material is a kind of brand-new nano particle super crystal lattice material, is beneficial to very much its application in the fields such as electronics and opto-electronic device, energy storage, catalysis.
Summary of the invention
The object of the present invention is to provide a kind of method simple, the method for what raw material was easy to get prepare three-dimensional high-sequential nano particle super crystal lattice material.
The method of preparation provided by the invention three-dimensional high-sequential nano particle super crystal lattice material, monodisperse nano metal oxide particle self-assembly is induced to be high-sequential superlattice by solvent evaporates, highly ordered mesosize pores material is obtained in conjunction with the process of high temperature cabonization acid etch, take mesoporous carbon as template, in its duct, required precursor species is filled by impregnating means, then by hydrolysis, pyrolysis, the means such as recrystallization impel presoma to decompose in the duct of mesoporous carbon, crosslinked/crystallization is to form the nano particle of respective substance, the crystalline structure of gained super crystal lattice material inherits crystalline structure and the spatial symmetry of initial metal oxide nanoparticles superlattice used.Concrete steps are as follows:
(1) using oleate as presoma, using oleic acid (or oleyl amine) as part, o is adopted to prepare monodisperse nano metal oxide particle, gained nanoparticle surface is coated by oleic acid (or oleyl amine) ligand molecular institute, and the particle diameter of nanoparticle and pattern can be modulated by modulation temperature, part consumption, solvent etc.; Above-mentioned nanoparticle is dissolved in non-polar solvent, forms stable metal oxide nanoparticles colloidal solution;
(2) gained metal oxide nanoparticles colloidal solution is placed in porcelain boat, control solvent evaporates speed, induced nano particles self assemble, namely obtains the nanoparticle superlattice with higher order structures after solvent volatilizees completely; It is carried out high-temperature calcination under nitrogen or argon, and oleic acid (or oleyl amine) ligand molecular of carbonization nanoparticle surface, obtains the metal oxide nanoparticles superlattice that carbon is coated;
(3) metal oxide nanoparticles super crystal lattice material coated for carbon is scattered in strong acid carries out etching processing, after removing metal oxide nanoparticles, obtain the meso-porous carbon material with high-specific surface area, three-dimensional pore passage structure continuously;
(4) take meso-porous carbon material as template, in its duct, required precursor species is filled by impregnating method, then impel presoma to decompose in the duct of meso-porous carbon material by methods such as hydrolysis, pyrolysis, recrystallizations, be cross-linked, crystallization, generate the nano particle of respective substance, to form super crystal lattice material.
In the present invention, the metal oxide described in step (1) is transition metal oxide, specifically can be selected from Fe
3o
4, MnO, CoO, MnFe
2o
4, CdO, CuO, CoFe
2o
4; The temperature of reaction of described o is 250 ~ 330 DEG C, and the reaction times is 0.5 ~ 2 hour; The concentration of oleic acid (or oleyl amine) is 1.5 ~ 4.5 mM, and reaction solvent used is hexadecylene, octyl ether, octadecylene, one or more combinations in icosa alkene; Gained metal oxide nanoparticles particle diameter is 5 ~ 50 nm; Described non-polar solvent is one or more combinations in normal hexane, octane, toluene, chloroform, zellon, tetrahydrofuran (THF).
In the present invention, the temperature of the high-temperature calcination described in step (2) is 300 ~ 600 DEG C, and the time of calcining is 60 ~ 180 minutes.
In the present invention, step (3) strong acid used is the one or more combination in concentrated hydrochloric acid, nitric acid, sulfuric acid, and etching temperature is 20 ~ 60 DEG C.
In the present invention, the precursor species described in step (4) is the one or more combination in alkoxide, organometallics, sucrose, sulphur, anhydrous chloride, phosphoric acid salt, nitrate.
Be be connected by wicket between adjacent nanoparticles in super crystal lattice material prepared by the inventive method, improve the intergranular effect of intercoupling, be beneficial to its application in electronics and the field such as opto-electronic device, catalysis.
Scanning electron microscope analysis
Fig. 1 is initial 10 nm Fe
3o
4nano particle superlattice become the coated Fe of carbon after 500 DEG C of calcinings
3o
4the scanning electron microscopic picture of nano particle superlattice.As can be seen from the figure, Fe
3o
4nanoparticle superlattice still can keep extraordinary pattern and have the crystalline structure of high-sequential after 500 DEG C of calcinings.
Fig. 2 is the scanning electron microscopic picture of the meso-porous carbon material after salt acid etch.Can obviously find out from figure, the carbon material after over etching has the orderly pore passage structure arrangement of structure height.Material after etching, no longer has magnetic, proves Fe
3o
4nanoparticle is etched is removed completely.
Fig. 3 is the scanning electron microscopic picture of the titania nanoparticles superlattice taking meso-porous carbon material as Template preparation.As can be seen from the figure, titanium dioxide nano-particle superlattice have the ordered 3 D structure of high-sequential.
Low-angle scattering of X-rays is analyzed
Fig. 4 take meso-porous carbon material as the low-angle scattering of X-rays figure of the titania nanoparticles superlattice of Template preparation, and different scattering peak represents different crystal faces, confirms the high-sequential pore passage structure of titania nanoparticles super crystal lattice material further.
TEM (transmission electron microscope) analysis
Fig. 5 is the transmission electron microscope picture of the carbon nano-particle superlattice taking meso-porous carbon material as Template preparation.As can be seen from the figure, carbon nano-particle superlattice have the ordered 3 D structure of high-sequential.
In sum, hinge structure of the present invention has following characteristics:
The present invention utilizes self-assembly transition metal oxide nano particle superlattice to be template, take oleic acid as carbon source, preparation has the mesoporous carbon nano material of high-sequential, three-dimensional continuous aperture structure, take mesoporous carbon as the nano particle super crystal lattice material of Template preparation many kinds of substance.The present invention has the following advantages, and gained nano particle super crystal lattice material has high-sequential, continuously adjustable particle diameter on the one hand; On the other hand, adjacent nanoparticles is connected by the window of 1-3 nm, and intergranular coupling strengthens greatly.Compared with the method preparing nano particle superlattice with tradition, this material preparation method is easy, and the nano particle super crystal lattice material that a lot of traditional method is difficult to realize simultaneously can be prepared by this method.
Accompanying drawing explanation
Fig. 1 is the coated Fe of carbon
3o
4the scanning electron microscope (SEM) photograph of nanoparticle superlattice.
Fig. 2 is the scanning electron microscope (SEM) photograph of meso-porous carbon material prepared by the present invention.
Fig. 3 is the scanning electron microscope (SEM) photograph of titania nanoparticles superlattice prepared by the present invention.
Fig. 4 is the X-ray small angle pattern spectrum of titania nanoparticles superlattice prepared by the present invention.
Fig. 5 is the transmission electron microscope picture of carbon nano-particle superlattice prepared by the present invention.
Embodiment
Embodiment 1
(1) Fe
3o
4the preparation of nanoparticle: be dissolved in 200 g octadecylenes by 36 g iron oleates and 5.7 g oleic acid, lower 320 DEG C of reaction 30 min of nitrogen protection, obtain the Fe of particle diameter 11 nm
3o
4nanoparticle, adds ethanol by nanoparticle precipitate out, after centrifugal, is dissolved in normal hexane by gained nanoparticle, and forming concentration is ~ 10 mg mL
-1stable colloidal solutions.
(2) Coated with Oleic Acid Fe
3o
4the preparation of nanoparticle superlattice: by gained Fe under room temperature
3o
4nanometer particle colloid solution is placed in porcelain boat, and under room temperature, normal hexane naturally volatilizees and obtains the Fe of high-sequential Coated with Oleic Acid completely
3o
4nanoparticle superlattice.
(3) the coated Fe of carbon
3o
4the preparation of nanoparticle superlattice: by Coated with Oleic Acid Fe
3o
4nanoparticle super crystal lattice material is transferred in tube furnace, and under nitrogen or argon gas atmosphere, 500 DEG C of high-temperature calcinations 2 hours, can obtain the coated Fe of carbon
3o
4nanoparticle superlattice, by coated for gained carbon Fe
3o
4nanoparticle super crystal lattice material is scattered in concentrated hydrochloric acid, and stirring at room temperature 24 h, etches away Fe
3o
4nanoparticle, namely obtains the meso-porous carbon material that aperture is about 10 nm.
(4) preparation of high-sequential tin oxide nano particles super crystal lattice material: gained 0.1 g meso-porous carbon material be impregnated in (1 M) in the aqueous isopropanol of isopropyl titanate, stir 6 h, by centrifugal, mesoporous carbon is separated, be exposed to air to be hydrolyzed by isopropyl titanate, dipping, centrifugal, hydrolytic process repetition twice acquisition titania nanoparticles super crystal lattice material.
Embodiment 2
(1) Fe
3o
4the preparation of nanoparticle: be dissolved in 200 g octadecylenes by 36 g iron oleates and 8.55 g oleic acid, lower 320 DEG C of reaction 30 min of nitrogen protection, obtain particle diameter 14 about nm Fe
3o
4nanoparticle.
(2) Coated with Oleic Acid Fe
3o
4the preparation of nanoparticle superlattice: with embodiment 1.
(3) preparation of highly ordered mesosize pores carbon material: with embodiment 1.
(4) preparation of high-sequential carbon nano-particle super crystal lattice material: gained 0.1 g meso-porous carbon material be impregnated in (1 M) in aqueous sucrose solution; add the 0.1 g vitriol oil; stir 6 h; by centrifugal, mesoporous carbon is separated; dry 1 h in 80 DEG C of vacuum drying ovens, dipping, centrifugal, drying process repetition twice, lower 500 DEG C of reaction 30 min of nitrogen protection; impel sucrose carbonization, obtain carbon nano-particle super crystal lattice material.
Embodiment 3
(1) Fe
3o
4the preparation of nanoparticle: be dissolved in 200 g hexadecylenes by 36 g iron oleates and 5.7 g oleic acid, lower 280 DEG C of reaction 30 min of nitrogen protection, obtain particle diameter 10 about nm Fe
3o
4nanoparticle.
(2) Coated with Oleic Acid Fe
3o
4the preparation of nanoparticle superlattice: with embodiment 1.
(3) preparation of highly ordered mesosize pores carbon material: with embodiment 1.
(4) preparation of high-sequential nano SiO 2 particle material: gained 0.1 g meso-porous carbon material be impregnated in (1 M) in the ethanolic soln of tetraethoxy, stir 6 h, by centrifugal, mesoporous carbon is separated, drip two ammonia solns, allow teos hydrolysis, dipping, centrifugal, hydrolytic process repeat twice and obtain nano SiO 2 particle super crystal lattice material.
Embodiment 4
(1) Fe
3o
4the preparation of nanoparticle: be dissolved in 200 g hexadecylenes by 36 g iron oleates and 5.7 g oleic acid, 320 DEG C of reaction 30 min, obtain the cube shaped Fe of particle diameter 10 about nm in air atmosphere
3o
4nanoparticle.
(2) Coated with Oleic Acid Fe
3o
4the preparation of nanoparticle superlattice: with embodiment 1.
(3) preparation of highly ordered mesosize pores carbon material: with embodiment 1.
(4) preparation of high-sequential titania nanoparticles super crystal lattice material: gained 0.1 g meso-porous carbon material be impregnated in anhydrous stannic chloride, stir 6 h, by centrifugal, mesoporous carbon is separated, be exposed to air to be hydrolyzed by tin tetrachloride, dipping, centrifugal, hydrolytic process repetition twice acquisition tin oxide nano particles super crystal lattice material.
Claims (5)
1. a preparation method for nano particle super crystal lattice material, is characterized in that concrete steps are as follows:
(1) using oleate as presoma, using oleic acid or oleyl amine as part, adopt o to prepare monodisperse nano metal oxide particle, gained nanoparticle surface by oleic acid or oleyl amine ligand molecular institute coated; Above-mentioned nanoparticle is dissolved in non-polar solvent, forms stable metal oxide nanoparticles colloidal solution;
(2) gained metal oxide nanoparticles colloidal solution is placed in porcelain boat, control solvent evaporates speed, induced nano particles self assemble, namely obtains the nanoparticle superlattice with higher order structures after solvent volatilizees completely; Nanoparticle superlattice are carried out high-temperature calcination under nitrogen or argon, the oleic acid of carbonization nanoparticle surface or oleyl amine ligand molecular, obtain the metal oxide nanoparticles superlattice that carbon is coated;
(3) metal oxide nanoparticles super crystal lattice material coated for carbon is scattered in strong acid carries out etching processing, after removing metal oxide nanoparticles, obtain the meso-porous carbon material with high-specific surface area, three-dimensional pore passage structure continuously;
(4) take meso-porous carbon material as template, in its duct, required precursor species is filled by dipping method, then by hydrolysis, pyrolysis or recrystallization method, presoma is decomposed in the duct of meso-porous carbon material, is cross-linked, crystallization, generate the nano particle of respective substance, thus form super crystal lattice material;
Metal oxide described in step (1) is selected from Fe
3o
4, MnO, CoO, MnFe
2o
4, CdO, CuO, CoFe
2o
4; The temperature of reaction of described o is 250 ~ 330 DEG C, about 0.5 ~ 2 hour reaction times.
2. the preparation method of nano particle super crystal lattice material according to claim 1, it is characterized in that the concentration of the oleic acid described in step (1) or oleyl amine is 1.5 ~ 4.5 mM, reaction solvent used is a kind of in hexadecylene, octyl ether, octadecylene, icosa alkene or wherein multiple; Gained metal oxide nanoparticles particle diameter is 5 ~ 50 nm; Described non-polar solvent is a kind of in normal hexane, octane, toluene, chloroform, zellon, tetrahydrofuran (THF) or wherein multiple.
3. the preparation method of nano particle super crystal lattice material according to claim 1, is characterized in that the temperature of the high-temperature calcination described in step (2) is 300 ~ 600 DEG C, and the time of calcining is 60 ~ 180 minutes.
4. the preparation method of nano particle super crystal lattice material according to claim 1, it is characterized in that strong acid used in step (3) is a kind of in concentrated hydrochloric acid, nitric acid, sulfuric acid or wherein several, etching temperature is 20 ~ 60 DEG C.
5. the preparation method of nano particle super crystal lattice material according to claim 1, is characterized in that the precursor species described in step (4) is a kind of in alkoxide, sucrose, sulphur, anhydrous chloride, phosphoric acid salt, nitrate or wherein several.
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