CN102408228A - Preparation method of synthetic series monodisperse rare earth-doped cobalt ferrite nanoparticle - Google Patents
Preparation method of synthetic series monodisperse rare earth-doped cobalt ferrite nanoparticle Download PDFInfo
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Abstract
Belonging to the technical field of inorganic material preparation technologies, the invention provides a preparation method of a synthetic series monodisperse rare earth-doped cobalt ferrite nanoparticle. The method comprises: step 1: adding a ferric salt, a cobalt salt and a rare earth salt into a high boiling organic solvent and mixing them uniformly so as to prepare a mixed solution with a total metal ion molar concentration of 0.02-0.2mol/L; step 2: adding a surfactant into the mixed solution, and raising the temperature for reaction under the protection of an inert gas; step 3: after the stop of the reaction, adding an excess polar solvent, conducting centrifugal separation and collecting the precipitate, which is then washed by ethanol and dried. The preparation method of a synthetic series monodisperse rare earth-doped cobalt ferrite nanoparticle in the invention can prepare a product with uniform particle size, good dispersibility and adjustable dimension, and has a milder reaction temperature than existing methods, thus being good for energy saving. The method of the invention is characterized by simple equipment, good technical repeatability, stable product quality, and easy amplification, thus boasting broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, belong to the inorganic compound semiconductor technical field of material.
Background technology
Ferrite Material is owing to have the resistivity height; Have characteristics such as higher magnetic permeability and cost be low in the microwave low-frequency range; Occupy critical role in space flight military project and civilian magnetic fields; It as absorbing material, can effectively be absorbed the hertzian wave with microwave frequency, improve the stealthy performance of weaponrys such as aircraft, tank, naval vessel, guided missile, torpedo.But, need to add other media usually its performance is improved because single ferrite work frequency band is very narrow.REE has the paired 4f electronic structure that is shielded by outermost electron, thereby their atom and ion have special electromagnetic performance.It is found that, when a certain amount of REE being added in the oxide compound of iron or manganese, can further improve the magnetic property and the absorbing property of Ferrite Material.Therefore, the synthetic and property research of rear-earth-doped vectolite material becomes the focus of broad research.
At present the used method of the preparation of rear-earth-doped vectolite material is mainly sol-gel method; Be that product passes through soluble metallic salt such as muriate or nitrate salt according to certain mixed dissolving; Solution is slowly evaporated obtain colloidal sol; Be dried to glue then, get through high-temperature roasting.Prepared rear-earth-doped vectolite nano-crystal film (J.Appl.Phys.85 volume, 2782 pages, 1999) like the Yan Chunhua of Peking University professor seminar through sol-gel method.Be respectively in the patent of CN101367647 and CN101452756A at publication number, the Huang Ying of Northwest University etc. utilizes sol-gel method to prepare lanthanum and mixes and the adulterated nano barium ferrite film of cerium.Yet, because this method needs higher temperature (more than 800 ℃) and long time (more than 12 hours) usually, be unfavorable for save energy, raise the efficiency.Simultaneously, because this method lacks effectively control to nucleating growth speed, mainly there are shortcomings such as size adjustable property difference and skewness in present resulting product, has influence on the performance and the application of material.It is evenly adjustable to develop a kind of size, good dispersivity, and product quality is stable, and the preparation method of good reproducibility is a major challenge that exists at present.
Summary of the invention
The objective of the invention is to the deficiency to prior art, provide a kind of equipment simple, be easy to realize to control, the preparation method of a kind of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles of the composition of good process repeatability, constant product quality and controllable size.
The present invention provides a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, adopts chemical solution method, specifically comprises following step:
Step 1: in high boiling organic solvent (purity is greater than 85%), add three kinds of different metallic salt; Be respectively molysite, cobalt salt and rare-earth salts and (be analytical pure; Promptly greater than 99.9%), stir, process the mixing solutions that the metals ion total mol concentration is 0.02～0.2mol/L; It is Co that the proportional range that adds between above-mentioned three kinds of metal-salts satisfies the metals ion mol ratio
2+: Fe
3+: RE
3+=1: (1.88～1.99): (0.01～0.12);
Described high boiling organic solvent is selected from a kind of in phenyl ether or the two Bian ethers.
Described three kinds of different metallic salt are the acetylacetonate or the benzoate of chosen from Fe, cobalt and rare earth respectively, wherein rare-earth salts satisfy with the rear-earth-doped vectolite that will prepare in rare earth identical.Like acetyl acetone iron (III), acetyl acetone cobalt (II) and phenylformic acid rare earth (III).
Step 2: wherein further add more than one tensio-active agents (CP), Fe in tensio-active agent and the mixing solutions to mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion molar ratio is 5～15, under the protection of rare gas element, is warming up to 200-350 ℃ of reaction 1-4h down.Said rare gas element is high-purity argon or high purity nitrogen.Tensio-active agent is preferably oleyl amine (CP), oleic acid (CP) or dodecanediol (CP).
Step 3: remove heating source after reaction stops, question response liquid cooling but back adds excessive polar solvent, and polar solvent comprises ethanol (analytical pure) or acetone (analytical pure); After stirring; The spinning collecting precipitation is placed on 40-60 ℃ of following drying in the baking oven with ethanol (analytical pure) washing (preferably washing more than 4 times), and 6～10 hours time of drying, products therefrom was a black powder; This black powder is a nano particle, and easy dissolving is scattered in the non-polar solvent.
Alr mode in the described step 3 can be the mode of magnetic agitation, mechanical stirring or ultrasonic concussion, and metal-salt is dispersed in the solvent.
The advantage that the present invention has is:
1, the present invention proposes a kind of preparation method of synthetic monodisperse rare earth doping cobalt ferrite nanoparticles, and the products therefrom particle diameter is even, good dispersivity, size adjustable;
2, the present invention proposes a kind of preparation method of synthetic monodisperse rare earth doping cobalt ferrite nanoparticles, and temperature of reaction is gentle than existing methods, helps save energy;
3, the present invention proposes a kind of preparation method of synthetic monodisperse rare earth doping cobalt ferrite nanoparticles, and wider range (200-350 ℃) can be selected arbitrarily according to practical situation and needs, and the condition of reaction is easy to control;
4, the present invention proposes a kind of preparation method of synthetic monodisperse rare earth doping cobalt ferrite nanoparticles, and equipment is simple, good process repeatability, constant product quality, is easy to amplify, and has comparatively wide application prospect.
Description of drawings
Fig. 1: preparing method's schema of a kind of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles provided by the invention;
Fig. 2: the transmission electron microscope photo of the embodiment of the invention 1 resulting gadolinium doping vectolite monodisperse nanoparticle;
Fig. 3: the transmission electron microscope photo of the embodiment of the invention 2 resulting gadolinium doping vectolite monodisperse nanoparticles;
Fig. 4: the transmission electron microscope photo of the embodiment of the invention 3 resulting gadolinium doping vectolite monodisperse nanoparticles;
Fig. 5: the transmission electron microscope photo of the embodiment of the invention 4 resulting europium doping vectolite monodisperse nanoparticles;
Fig. 6: the transmission electron microscope photo of the embodiment of the invention 5 resulting samarium doping vectolite monodisperse nanoparticles;
Fig. 7: the transmission electron microscope photo of the embodiment of the invention 6 resulting gadolinium doping vectolite monodisperse nanoparticles;
Fig. 8: different REEs are mixed at the x-ray diffraction pattern that obtains synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles among the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
The present invention provides a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, adopts chemical solution method, and is as shown in Figure 1, specifically comprises following step:
Step 1: in high boiling organic solvent (purity is greater than 85%), add three kinds of different metallic salt; Be respectively molysite, cobalt salt and rare-earth salts and (be analytical pure; Promptly greater than 99.9%), stir, process the mixing solutions that the metals ion total mol concentration is 0.02～0.2mol/L; It is Co that the proportional range that adds between above-mentioned three kinds of metal-salts satisfies the metals ion mol ratio
2+: Fe
3+: RE
3+=1: (1.88～1.99): (0.01～0.12);
Described high boiling organic solvent is selected from a kind of in phenyl ether or the two Bian ethers.
Described three kinds of different metallic salt are the acetylacetonate or the benzoate of chosen from Fe, cobalt and rare earth respectively, wherein rare-earth salts satisfy with the rear-earth-doped vectolite that will prepare in rare earth identical.Like acetyl acetone iron (III), acetyl acetone cobalt (II) and phenylformic acid rare earth (III).
Step 2: wherein further add more than one tensio-active agents (CP), Fe in tensio-active agent and the mixing solutions to mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion mol ratio is 5～15, forms the reddish-brown homogeneous solution, under the protection of rare gas element, is warming up to 200-350 ℃ of reaction 1-4h down.Said rare gas element is high-purity argon or high purity nitrogen.Tensio-active agent is preferably oleyl amine (CP), oleic acid (CP) or dodecanediol (CP).When the tensio-active agent that adds when being two or more, the amount between each tensio-active agent is restriction not, only needs the tensio-active agent total amount to satisfy 5～15 with total metals ion mol ratio and gets final product.
Step 3: remove heating source after reaction stops, question response liquid cooling but back adds excessive polar solvent, and polar solvent comprises ethanol or acetone (analytical pure); After stirring; The spinning collecting precipitation is placed on 40-60 ℃ of following drying in the baking oven with ethanol (analytical pure) washing (preferably washing more than 4 times), and 6～10 hours time of drying, products therefrom was a black powder; This black powder is a nano particle, and easy dissolving is scattered in the non-polar solvent.Said alr mode can be the mode of magnetic agitation, mechanical stirring or ultrasonic concussion, and metal-salt is dispersed in the solvent.
In preparation method of the present invention, oleic acid and oleyl amine have been wrapped up in the surface of rear-earth-doped vectolite nanoparticle, therefore have hydrophobicity.After adding polar solvent, rear-earth-doped vectolite nanoparticle can not be scattered in the polar solvent, can rear-earth-doped vectolite nanoparticle be separated through centrifugation method, reaches the purpose of the rear-earth-doped vectolite nanoparticle of washing.In the present invention, can repeatedly add polar solvent,, repeatedly wash rear-earth-doped vectolite nanoparticle, to guarantee to obtain comparatively purified rear-earth-doped vectolite nanoparticle through the method for spinning repeatedly.
In preparation method of the present invention, the metals ion total mol concentration is 0.02～0.2mol/L, and different concentration has considerable influence to the particle diameter of product.As shown in Figure 2; Select phenyl ether when high boiling organic solvent, when consumption was 20mL, the particle diameter of resulting gadolinium doping vectolite nanoparticle was 7～8nm; And it is as shown in Figure 7; Be consistent in other conditions, when only the phenyl ether consumption being increased to 60mL, the particle diameter of resulting gadolinium doping vectolite nanoparticle is reduced to 3～4nm.
Embodiment 1:
Present embodiment provides a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, specifically comprises following step:
Step 1: in 20ml phenyl ether (purity is greater than 85%), add 1.97mmol acetyl acetone iron (III), 1.00mmol acetyl acetone cobalt (II) and 0.03mmol phenylformic acid gadolinium (III) and (be analytical pure; Be that purity is greater than 99.9%); Stir, process the mixing solutions that the metals ion total mol concentration is 0.15mol/L;
Step 2: wherein further add 6.0mmol dodecanediol, 6.0mmol oleic acid and 6.0mmol oleyl amine (being CP), Fe in tensio-active agent and the mixing solutions to mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion mol ratio is 6, under the protection of rare gas element high-purity argon, is warming up to 250 ℃ of reaction 3h down.Said rare gas element is high-purity argon or high purity nitrogen.
Step 3: remove heating source after reaction stops; The question response liquid cooling is the excess ethanol solution (analytical pure) of back adding 100mL but, after stirring, and the spinning collecting precipitation; Be placed on for 4 times in the baking oven dry under 40 ℃ with ethanolic soln (analytical pure) washing; 10 hours time of drying, products therefrom was a black powder, and this black powder is a nano particle, and easy dissolving is scattered in the non-polar solvent.
The synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles for preparing is 1% gadolinium doping vectolite monodisperse nanoparticle for the gadolinium molar content; Like Fig. 2; The even size distribution of prepared gadolinium doping vectolite nanoparticle, particle diameter is at 7～8nm.
Embodiment 2:
The embodiment of the invention provides a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, specifically comprises following step:
Step 1: in the 20.0ml phenyl ether, add 1.94mmol acetyl acetone iron (III), 1.00mmol acetyl acetone cobalt (II) and 0.06mmol phenylformic acid gadolinium (III) in (purity is greater than 85%) and (be analytical pure; Promptly greater than 99.9%); Stir, process the mixing solutions that the metals ion total mol concentration is 0.15mol/L;
Step 2: wherein further add 6.0mmol dodecanediol, 6.0mmol oleic acid, 6.0mmol oleyl amine (being CP), Fe in tensio-active agent and the mixing solutions to mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion mol ratio is 6, forms the reddish-brown homogeneous solution, under the protection of rare gas element high-purity argon, is warming up to 250 ℃ of reaction 3h down.
Step 3: remove heating source after reaction stops; The question response liquid cooling is the excess ethanol solution (analytical pure) of back adding 100mL but, after stirring, and the spinning collecting precipitation; Be placed on for 4 times in the baking oven dry under 40 ℃ with ethanolic soln (analytical pure) washing; 10 hours time of drying, products therefrom was a black powder, and this black powder is a nano particle, and easy dissolving is scattered in the non-polar solvent.
The synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles for preparing is 2% gadolinium doping vectolite monodisperse nanoparticle for the gadolinium molar content; Like Fig. 3; The even size distribution of prepared gadolinium doping vectolite nanoparticle, particle diameter is at 7～8nm.
Embodiment 3:
The embodiment of the invention provides a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, specifically comprises following step:
Step 1: in 20.0mL phenyl ether (purity is greater than 85%), add 1.88mmol acetyl acetone iron (III), 1.00mmol acetyl acetone cobalt (II) and 0.12mmol phenylformic acid gadolinium (III) and (be analytical pure; Promptly greater than 99.9%); Stir, process the mixing solutions that the metals ion total mol concentration is 0.15mol/L;
Step 2: wherein further add 6.0mmol dodecanediol, 6.0mmol oleic acid, 6.0mmol oleyl amine (being CP), Fe in tensio-active agent and the mixing solutions to mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion mol ratio is 6, forms the reddish-brown homogeneous solution, under the protection of rare gas element high-purity argon, is warming up to 250 ℃ of reaction 3h down.
Step 3: remove heating source after reaction stops; The question response liquid cooling is the excess ethanol solution (analytical pure) of back adding 100mL but, after stirring, and the spinning collecting precipitation; Be placed on for 4 times in the baking oven dry under 40 ℃ with ethanolic soln (analytical pure) washing; 10 hours time of drying, products therefrom was a black powder, and this black powder is a nano particle, and easy dissolving is scattered in the non-polar solvent.
The synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles for preparing is 4% gadolinium doping vectolite monodisperse nanoparticle for the gadolinium molar content; Like Fig. 4; The even size distribution of prepared gadolinium doping vectolite nanoparticle, particle diameter is at 7～8nm.
Embodiment 4:
The embodiment of the invention provides a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, specifically comprises following step:
Step 1: in 20.0mL phenyl ether (purity is greater than 85%), add 1.94mmol acetyl acetone iron (III), 1.00mmol acetyl acetone cobalt (II) and 0.06mmol phenylformic acid europium (III) and (be analytical pure; Promptly greater than 99.9%); Stir, process the mixing solutions that the metals ion total mol concentration is 0.15mol/L;
Step 2: wherein further add 6.0mmol dodecanediol, 6.0mmol oleic acid and 6.0mmol oleyl amine (being CP), Fe in tensio-active agent and the mixing solutions to mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion mol ratio is 6, forms the reddish-brown homogeneous solution, under the protection of rare gas element high-purity argon, is warming up to 250 ℃ of reaction 3h down.
Step 3: remove heating source after reaction stops; The question response liquid cooling is the excess ethanol solution (analytical pure) of back adding 100mL but, after stirring, and the spinning collecting precipitation; Be placed on for 4 times in the baking oven dry under 40 ℃ with ethanolic soln (analytical pure) washing; 10 hours time of drying, products therefrom was a black powder, and this black powder is a nano particle, and easy dissolving is scattered in the non-polar solvent.
The synthesizing series list dispersion europium doping cobalt ferrite nanoparticles for preparing is 2% europium doping vectolite monodisperse nanoparticle for the europium molar content; Like Fig. 5; The even size distribution of prepared europium doping vectolite nanoparticle, particle diameter is at 14～15nm.
Embodiment 5:
The embodiment of the invention provides a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, specifically comprises following step:
Step 1: in 20.0mL phenyl ether (purity is greater than 85%), add 1.94mmol acetyl acetone iron (III), 1.00mmol acetyl acetone cobalt (II) and 0.06mmol phenylformic acid samarium (III) and (be analytical pure; Promptly greater than 99.9%); Stir, process the mixing solutions that the metals ion total mol concentration is 0.15mol/L;
Step 2: wherein further add 6.0mmol dodecanediol, 6.0mmol oleic acid, 6.0mmol oleyl amine (being CP), Fe in tensio-active agent and the mixing solutions to mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion mol ratio is 6, forms the reddish-brown homogeneous solution, under the protection of rare gas element high-purity argon, is warming up to 250 ℃ of reaction 3h down.
Step 3: remove heating source after reaction stops; The question response liquid cooling is the excess ethanol solution (analytical pure) of back adding 100mL but, after stirring, and the spinning collecting precipitation; Be placed on for 4 times in the baking oven dry under 40 ℃ with ethanolic soln (analytical pure) washing; 10 hours time of drying, products therefrom was a black powder, and this black powder is a nano particle, and easy dissolving is scattered in the non-polar solvent.
The synthesizing series list dispersion samarium doping cobalt ferrite nanoparticles for preparing is 2% samarium doping vectolite monodisperse nanoparticle for the samarium molar content; Like Fig. 6; The even size distribution of prepared samarium doping vectolite nanoparticle, particle diameter is at 8～9nm.
Embodiment 6:
The embodiment of the invention provides a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, specifically comprises following step:
Step 1: in 60.0mL phenyl ether (purity is greater than 85%), add 1.97mmol acetyl acetone iron (III), 1.00mmol acetyl acetone cobalt (II) and 0.03mmol phenylformic acid gadolinium (III) and (be analytical pure; Promptly greater than 99.9%); Stir, process the mixing solutions that the metals ion total mol concentration is 0.05mol/L;
Step 2: wherein further add 6.0mmol dodecanediol, 6.0mmol oleic acid, 6.0mmol oleyl amine (being CP), Fe in tensio-active agent and the mixing solutions to mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion mol ratio is 6, forms the reddish-brown homogeneous solution, under the protection of rare gas element high-purity argon, is warming up to 250 ℃ of reaction 3h down.
Step 3: remove heating source after reaction stops; The question response liquid cooling is the excess ethanol solution (analytical pure) of back adding 100mL but, after stirring, and the spinning collecting precipitation; Be placed on for 4 times in the baking oven dry under 40 ℃ with ethanolic soln (analytical pure) washing; 10 hours time of drying, products therefrom was a black powder, and this black powder is a nano particle, and easy dissolving is scattered in the non-polar solvent.
The synthesizing series list dispersion gadolinium doping cobalt ferrite nanoparticles for preparing is 1% gadolinium doping vectolite monodisperse nanoparticle for the gadolinium molar content; Like Fig. 7; The even size distribution of prepared gadolinium doping vectolite nanoparticle, particle diameter is at 3～4nm.
In preparation method of the present invention, the metals ion total mol concentration is 0.02～0.2mol/L, and different concentration has considerable influence to the particle diameter of product.As shown in Figure 2; Select phenyl ether when high boiling organic solvent, when consumption was 20mL, the particle diameter of resulting gadolinium doping vectolite nanoparticle was 7～8nm; And it is as shown in Figure 7; Be consistent in other conditions, when only the phenyl ether consumption being increased to 60mL, the particle diameter of resulting gadolinium doping vectolite nanoparticle is reduced to 3～4nm.It is as shown in Figure 8 that the different REEs of the present invention are mixed the x-ray diffraction pattern of the synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles that each embodiment obtains; As can be seen from the figure; The x-ray diffraction pattern of product is corresponding consistent with the vectolite of spinel structure (JCPDS No.22-1086); Do not observe the diffraction peak from rare earth and rare earth oxide, this shows does not have dephasign to generate, and rare earth ion has been incorporated in the lattice of vectolite fully.
Embodiment 7:
The embodiment of the invention provides a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, specifically comprises following step:
Step 1: in two Bian ethers (purity is greater than 85%), add three kinds of different metallic salt; Be respectively acetyl acetone iron (III), cobalt salt and phenylformic acid gadolinium (III) and (be analytical pure; Promptly greater than 99.9%), stir, process the mixing solutions that the metals ion total mol concentration is 0.2mol/L; It is Co that the proportional range that adds between above-mentioned three kinds of metal-salts satisfies the metals ion mol ratio
2+: Fe
3+: RE
3+=1: 1.99: 0.01;
Step 2: wherein further add oleyl amine (CP) and oleic acid (CP) to mixing solutions, oleyl amine and oleic mol ratio are 1: 2, Fe in oleyl amine (CP) and oleic acid (CP) and the mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion molar ratio is 15, under the protection of rare gas element high-purity argon, is warming up to 350 ℃ of reaction 4h down.
Step 3: remove heating source after reaction stops; Question response liquid cooling but back adds excessive propanone (analytical pure); After stirring, the spinning collecting precipitation is placed on for 5 times in the baking oven dry under 60 ℃ with ethanol (analytical pure) washing; 10 hours time of drying, products therefrom was a black powder, and this nano particle is prone to dissolving and is scattered in the non-polar solvent.
Embodiment 8:
The embodiment of the invention provides a kind of preparation method of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles, specifically comprises following step:
Step 1: in two Bian ethers (purity is greater than 85%), add three kinds of different metallic salt; Be respectively acetyl acetone iron (III), cobalt salt and phenylformic acid gadolinium (III) and (be analytical pure; Promptly greater than 99.9%), stir, process the mixing solutions that the metals ion total mol concentration is 0.2mol/L; It is Co that the proportional range that adds between above-mentioned three kinds of metal-salts satisfies the metals ion mol ratio
2+: Fe
3+: RE
3+=1: 1.95: 0.05;
Step 2: wherein further add oleic acid (CP) to mixing solutions, Fe in oleic acid (CP) and the mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion molar ratio is 10, under the protection of rare gas element high-purity argon, is warming up to 300 ℃ of reaction 2h down.
Step 3: remove heating source after reaction stops; Question response liquid cooling but back adds excessive propanone (analytical pure); After stirring, the spinning collecting precipitation is placed on for 3 times in the baking oven dry under 50 ℃ with ethanol (analytical pure) washing; 8 hours time of drying, products therefrom was a black powder, and this nano particle is prone to dissolving and is scattered in the non-polar solvent.
Claims (7)
1. the preparation method of a synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles is characterized in that: comprise following step:
Step 1: in high boiling organic solvent, add three kinds of different metallic salt, be respectively molysite, cobalt salt and rare-earth salts, stir, process the mixing solutions that the metals ion total mol concentration is 0.02～0.2mol/L; It is Co that the proportional range that adds between above-mentioned three kinds of metal-salts satisfies the metals ion mol ratio
2+: Fe
3+: RE
3+=1: (1.88～1.99): (0.01～0.12);
Step 2: wherein further add more than one tensio-active agents, Fe in tensio-active agent and the mixing solutions to mixing solutions
3+, Co
2+And RE
3+Constituting total metals ion mol ratio is 5～15, forms the reddish-brown homogeneous solution, under the protection of rare gas element, is warming up to 200～350 ℃ of reaction 1-4h down;
Step 3: remove heating source after reaction stops; Question response liquid cooling but back adds excessive polar solvent; After stirring, the spinning collecting precipitation is placed in the baking oven dry under 40-60 ℃ with washing with alcohol; 6～10 hours time of drying, obtain synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles.
2. the preparation method of a kind of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles according to claim 1 is characterized in that: the high boiling organic solvent in the described step 1 is selected from a kind of in phenyl ether or the two Bian ethers.
3. the preparation method of a kind of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles according to claim 1 is characterized in that: three kinds of different metallic salt in the described step 1 are respectively acetyl acetone iron, acetyl acetone cobalt and phenylformic acid rare earth.
4. the preparation method of a kind of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles according to claim 1 is characterized in that: rare gas element is high-purity argon or high purity nitrogen in the described step 2.
5. the preparation method of a kind of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles according to claim 1 is characterized in that: tensio-active agent is oleyl amine, oleic acid or dodecanediol in the described step 2.
6. the preparation method of a kind of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles according to claim 1 is characterized in that: described step 3 Semi-polarity solvent is ethanolic soln or acetone soln.
7. the preparation method of a kind of synthesizing series monodisperse rare earth doping cobalt ferrite nanoparticles according to claim 1 is characterized in that: alr mode is magnetic agitation, mechanical stirring or ultrasonic concussion in the described step 3.
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| CN114084910A (en) * | 2021-10-15 | 2022-02-25 | 闽都创新实验室 | Cerium-nickel-cobalt-doped ferrite nano material and preparation method and application thereof |
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| CN105233968B (en) * | 2015-06-17 | 2017-11-14 | 陶栋梁 | A kind of method for separating different-grain diameter nano-particle |
| CN114084910A (en) * | 2021-10-15 | 2022-02-25 | 闽都创新实验室 | Cerium-nickel-cobalt-doped ferrite nano material and preparation method and application thereof |
| CN114084910B (en) * | 2021-10-15 | 2023-12-05 | 闽都创新实验室 | Cerium-nickel-cobalt doped ferrite nano material and preparation method and application thereof |
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