CN106315684B - The preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size - Google Patents
The preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the controllable spherical MnZn ferrite magnetic nano particle of size, include the following steps: that (1) will contain Fe respectively3+、Mn2+、Zn2+Salt be dissolved in the dicyandiamide solution based on ethylene glycol, form orange-yellow uniform mixed liquor；(2) coating material, sodium acetate are added in the mixed liquor that step (1) obtains, then magnetic agitation is ultrasonically treated, reaction kettle is heated at 160-200 DEG C, reacts 12-20h or more；(3) after reaction kettle is cooling, then wash products are dried in a vacuum drying oven, obtain black magnetic product；The present invention uses hydro-thermal method, by using the coating material of the different dicyandiamide solutions based on ethylene glycol and variety classes, dosage, realize to nano particle average grain diameter 30-350nm wide scope regulation.The magnetic nanoparticle regular appearance, size be distributed it is uniform, with excellent magnetic property.
Description
Technical field
The invention belongs to field of nanometer technology, it is related to a kind of spherical MnZn ferrite magnetic nano particle that size is controllable
Preparation method.
Background technique
In recent years, magnetic nanoparticle is in terms of biomedical applications such as MRI, tumor thermotherapy, target drug-carrying, biology biography
Sense, bio-separation etc. research are in widespread attention.This, which is primarily due to magnetic nanoparticle, has unique and excellent object
Reason, chemical property have magnetic responsiveness and superparamagnetism if partial size is small, large specific surface area, coupling capacity height, can be constant
Assemble under magnetic field and position, the electromagnetic wave absorption heat production under alternating magnetic field.In all kinds of magnetic nanoparticles, Fe3O4It is to be so far
The only magnetic nanoparticle of domestic and foreign scholars' most study.To preparation high dispersive, size is controllable, Fe of good biocompatibility3O4Magnetic
Property nano particle has carried out a large amount of research.But due to Fe3O4In there are Fe2+In metastable state, it is easy to lose an electricity again
Son becomes Fe3+Reach most stable of oxidation state, so as to cause the reduction of magnetic-particle magnetic property.In order to improve the anti-of magnetic-particle
Oxidation susceptibility, in recent years, a few studies person is by the substitution such as Mn, Zn, Co, Ni, Primary Study MnFe2O4、MnxZn1-xFe2O4、
CoFe2O4Equal ferrite magnetic nanos particle has higher saturation magnetization and better temperature rise effect.
MnZn ferrite magnetic nano particle is a kind of soft magnetic ferrite of widely used spinel structure, is had
The advantageous properties such as saturation magnetization height, easy magnetization, low-coercivity, good bioactivity, thus urged in biomedical, light
The fields such as change, aerospace flight technology have broad application prospects.Thus prepare the MnZn ferrimagnetism of different size and shapes
Nano particle is current research emphasis with the application demand for meeting different field.In addition, dimensional homogeneity can be to nano particle
Performance is such as magnetic, biocompatibility generates strong influence, therefore is also to need the weight considered in magnetic nanoparticle application
Want factor.
Existing MnZn ferrite magnetic nano preparation method of granules is complex, and the MnZn ferrite magnetic prepared
The size of property nano particle is inhomogenous.How to prepare that size is controllable, uniform MnZn ferrimagnetism using simple method
Nano particle is still the emphasis that everybody studies.
Summary of the invention
It is an object of the present invention to provide a kind of preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size, solutions
The controllable MnZn ferrite magnetic nano particle size of certainly existing method preparation size is inhomogenous, operating process is complicated asks
Topic.
The technical solution of the present invention is as follows: the preparation method of the spherical MnZn ferrite magnetic nano particle of size controllably, packet
Include following steps:
(1) preparation of precursor liquid is reacted
Fe will be contained respectively3+、Mn2+、Zn2+Salt be dissolved in the dicyandiamide solution based on ethylene glycol, magnetic force stirs at room temperature
It mixes, forms orange-yellow uniform mixed liquor；
(2) generation of spherical shape MnZn ferrite magnetic nano particle
Coating material, sodium acetate are added in the mixed liquor that step (1) obtains, then magnetic agitation carries out at ultrasound
It manages, is transferred in reaction kettle and seals after ultrasonic treatment, reaction kettle is heated at 160-200 DEG C, react 12-20h or more；
(3) post-processing of product
After reaction kettle is cooling, then wash products are dried in a vacuum drying oven, obtain black magnetic product；
The dicyandiamide solution based on ethylene glycol is ethylene glycol and tetraethylene-glycol, ethylene glycol and a contracting diethyl two
One of alcohol, ethylene glycol and water.
The coating material is polyethylene glycol (PEG), in polyvinylpyrrolidone (PVP), polyethyleneimine (PEI)
The mixing of a kind of or polyethylene glycol and polyvinylpyrrolidone or the mixing of polyethylene glycol and polyethyleneimine.
Further, Fe3+、Mn2+、Zn2+, sodium acetate molar ratio be 0.5:0.5:2:8.
Further, the relative molecular mass point of polyethylene glycol in step (2), polyvinylpyrrolidone, polyethyleneimine
It Wei 6000,10000,10000, Mn2+Molar ratio with polyethylene glycol, polyvinylpyrrolidone, polyethyleneimine is respectively
7.5-75、12.5-125、12.5-125。
Further, the volume ratio of ethylene glycol and tetraethylene-glycol is 1:1-3:1, ethylene glycol and diglycol
Volume ratio are as follows: the volume ratio 1:1-3:1 of 1:1-3:1, ethylene glycol and water.
Further, in step (3), the method for wash products are as follows: cleaned 4-5 times using alcohol and deionized water.
Further, in step (3), the temperature of drying is 70 DEG C.
Further, in step (1), Fe3+、Mn2+、Zn2+Salt be respectively FeCl3.6H2O、MnCl2.4H2O、ZnCl2。
Further, when dicyandiamide solution is ethylene glycol and water, Mn2+When molar ratio with PEG is 7.5, prepared nanometer
Mean particle size is 30nm；When dicyandiamide solution is ethylene glycol and tetraethylene-glycol, Mn2+When molar ratio with PEG is 7.5,
Prepared nano particle average grain diameter is 120nm；When dicyandiamide solution is ethylene glycol and diglycol, Mn2+With rubbing for PEI
When you are than being 12.5, prepared nano particle average grain diameter is 230nm；When dicyandiamide solution is ethylene glycol and a contracting diethyl two
Alcohol, Mn2+When being respectively 15,25 with the molar ratio of PEG and PEI, prepared nano particle average grain diameter is 240nm；Work as solvent
System is ethylene glycol and diglycol, Mn2+When molar ratio with PVP is 12.5, prepared nano particle average grain diameter
For 280nm；When dicyandiamide solution is ethylene glycol and diglycol, Mn2+When being respectively 15,25 with the molar ratio of PEG and PVP,
Prepared nano particle average grain diameter is 330nm；When dicyandiamide solution is ethylene glycol and diglycol, Mn2+With rubbing for PEG
When you are than being 7.5, prepared nano particle average grain diameter is 350nm.By using the different solvents based on ethylene glycol
The coating material of system and variety classes, dosage, average grain diameter regulate and control within the scope of 30-350nm.
The invention has the following advantages over the prior art:
The hydro-thermal method of the different solvents system provided by the invention based on ethylene glycol is used to prepare MnZn magnetic Nano
Grain, may be implemented to nano particle diameter 30-350nm range regulation.Prepared MnZn magnetic nanoparticle is spherical in shape,
Its pattern is uniform, uniform particle diameter, has good magnetic property；It contracts in ethylene glycol and tetraethylene-glycol system or ethylene glycol and one
The advantages such as the nano particle synthesized in diethylene glycol system has the intensity of magnetization high, and coercivity, Ms/Mr are low.The advantages of this method
It is that preparation process is simple, preparation condition is mild；Preparation process is controllable, reproducible；It can control by controlling dicyandiamide solution
The partial size of nano particle, magnetic property.This method has bright prospects in the fields such as industry and biologic applications.
Detailed description of the invention
Different solvents system of the Fig. 1 based on ethylene glycol, PEG are obtained magnetism after coating material (1g) hydro-thermal reaction
The XRD spectrum of nano particle.Dicyandiamide solution is respectively as follows: (a) ethylene glycol and water, (b) ethylene glycol and tetraethylene-glycol, (c) second
Two pure and mild diglycols；
It is solvent as dicyandiamide solution that Fig. 2, which is using ethylene glycol and diglycol, is repaired using the surface of variety classes, dosage
The XRD spectrum of the magnetic nanoparticle obtained after decorations agent hydro-thermal reaction: (d) PEI-1g, (e) PVP-1g, (f) PEG/PVP-
0.5g/0.5g。
Fig. 3 is the magnetism obtained after different solvents system (PEG is coating material: 1g) hydro-thermal reaction based on ethylene glycol
The hysteresis loop figure of nano particle.Dicyandiamide solution is respectively as follows: (a) ethylene glycol and water, (b) ethylene glycol and tetraethylene-glycol, (c)
Ethylene glycol and diglycol.
Fig. 4 is different solvents system (PEG is coating material: 1g) and the variety classes, dosage based on ethylene glycol
The magnetic nanoparticle scanning electricity obtained after coating material (ethylene glycol and diglycol be dicyandiamide solution) hydro-thermal reaction
Mirror SEM figure.(a) ethylene glycol and water, amplification factor are 160,000 times；(b) ethylene glycol and tetraethylene-glycol, amplification factor are 160,000
Times；(c) PEI-1g, amplification factor are 80,000 times；(d) PVP-1g, amplification factor are 80,000 times；(e)PEG/PVP-0.5g/0.5g,
Amplification factor is 80,000 times；(f) ethylene glycol and diglycol, amplification factor are 80,000 times.
Specific embodiment
Embodiment 1
Weigh 1.35g FeCl3.6H2O、0.247g MnCl2.4H2O、0.17g ZnCl2Be dissolved in 40mL ethylene glycol and
In the mixed solvent system of water, magnetic agitation 30min, forms orange-yellow uniform mixed liquor at room temperature.By the polyethylene glycol of 1g
(PEG), 3.6g anhydrous sodium acetate is added in the mixed liquor stirred evenly, magnetic agitation about 30min, then is carried out to mixed liquor
The ultrasonic treatment of about 10min.Mixed liquor is moved in the reaction kettle of the polytetrafluoroethyllining lining of 100ml and is sealed.By reaction kettle
It puts into baking oven, in 200 DEG C of reaction 12h.After reaction kettle is cooling, with alcohol and deionized water wash products 4-5 times, then exist
It is dried 70 DEG C in vacuum oven, under 8h, obtains black magnetic product.
Characterization: the nano particle prepared in ethylene glycol and aqueous solvent shown in (a) and Fig. 4 (a) as shown in figure 1
XRD spectrum and scanning electron microscope (SEM) photograph are it is found that prepared MnZn ferrite nanometer particle is spinel-type, and crystallization degree is higher,
Crystal form is good；There is not small nanoparticle agglomerates formation spherical nanoparticle in prepared nano particle in the dicyandiamide solution
The phenomenon that, and it is the spherical nanoparticle of single dispersion, complete crystallization.Through nanomeasure particle diameter distribution software statistics meter
It calculates, average grain diameter is about 30nm, and the standard deviation of partial size is small, and particle diameter distribution is relatively narrow, morphological rules.
Performance: the nano particle prepared in ethylene glycol and aqueous solvent shown in (a) in Fig. 3 is at room temperature 300k
Hysteresis loop it is found that the MnZn ferrite nanometer particle have soft magnetic characteristic.Remanent magnetism Mr is 19emu/g, and coercivity H is
162Oe.In addition, the saturation magnetization Ms of sample reaches 59.45emu/g, Mr/Ms 0.32.
Embodiment 2
Weigh 1.35g FeCl3.6H2O、0.247g MnCl2.4H2O、0.17g ZnCl2Be dissolved in 40mL ethylene glycol and
In the mixed solvent system of tetraethylene-glycol, magnetic agitation 30min, forms orange-yellow uniform mixed liquor at room temperature.By 1g
Polyethylene glycol (PEG), 3.6g anhydrous sodium acetate be added in the mixed liquor stirred evenly, magnetic agitation about 30min, then right
The ultrasonic treatment of mixed liquor progress about 10min.Mixed liquor is moved to close in the reaction kettle of the polytetrafluoroethyllining lining of 100ml
Envelope.Reaction kettle is put into baking oven, in 200 DEG C of reaction 12h.After reaction kettle is cooling, with alcohol and deionized water wash products
4-5 times, then in a vacuum drying oven 70 DEG C, dry under 8h, obtain black magnetic product.
Characterization: what is prepared in the dicyandiamide solution of ethylene glycol and tetraethylene-glycol as shown in Fig. 1 (b) and Fig. 4 (b) receives
XRD spectrum and the scanning electron microscope (SEM) photograph of rice grain are it is found that prepared MnZn ferrite nanometer particle is spinel-type, and crystallizes journey
Degree is higher, and crystal form is good；Minimum nanoparticle agglomerates form the big nano particle of uniform-spherical, and big nano particle point
It is preferable to dissipate property.It is calculated through nanomeasure particle diameter distribution software statistics, average grain diameter is about 120nm, and particle diameter distribution is equal
One, morphological rules.
Performance: the nano particle prepared in ethylene glycol and tetraethylene-glycol dicyandiamide solution as shown in Fig. 3 (a) is in room
It is found that the remanent magnetism Mr of the MnZn ferrite nanometer particle is 23emu/g, coercivity H 111Oe has hysteresis loop under temperature
Soft magnetic characteristic.In addition, the saturation magnetization Ms of sample reaches 70emu/g, Mr/Ms 0.329.
Embodiment 3
Weigh 1.35g FeCl3.6H2O、0.247g MnCl2.4H2O、0.17g ZnCl2Be dissolved in 40mL ethylene glycol and
In the dicyandiamide solution of diglycol, magnetic agitation 30min, forms orange-yellow uniform mixed liquor at room temperature.By the poly- of 1g
Ethylene glycol (PEG), 3.6g anhydrous sodium acetate are added in the mixed liquor stirred evenly, magnetic agitation about 30min, then to mixing
The ultrasonic treatment of liquid progress about 10min.Mixed liquor is moved in the reaction kettle of the polytetrafluoroethyllining lining of 100ml and is sealed.It will
Reaction kettle is put into baking oven, in 180 DEG C of reaction 16h.After reaction kettle is cooling, with alcohol and deionized water wash products 4-5 times,
Then in a vacuum drying oven 70 DEG C, dry under 8h, obtain black magnetic product.
Characterization: what is prepared in ethylene glycol and diglycol dicyandiamide solution shown in (c) and Fig. 4 (f) as shown in figure 1 receives
XRD spectrum and the scanning electron microscope (SEM) photograph of rice grain are it is found that prepared MnZn ferrite nanometer particle is spinel-type, and crystallizes journey
Degree is higher, and crystal form is good；Minimum nanoparticle agglomerates form the big nano particle of uniform-spherical.Its average grain diameter is about
350nm, particle diameter distribution is uniform, and only the grain diameter of only a few is 400nm, morphological rules, good dispersion.And it is closed in the system
At small nano particle partial size it is smaller than being synthesized in ethylene glycol and tetraethylene-glycol and ethylene glycol and aqueous solvent
The partial size of nano particle is small.
Performance: the nano particle prepared in ethylene glycol and diglycol dicyandiamide solution shown in (c) in Fig. 3 exists
It is found that the remanent magnetism Mr of MnZn ferrite nanometer particle is 15emu/g, coercivity H 102Oe has hysteresis loop at room temperature
Soft magnetic characteristic.In addition, the saturation magnetization Ms of sample reaches 76.35emu/g, Mr/Ms 0.196.
Embodiment 4
Weigh 1.35g FeCl3.6H2O、0.247g MnCl2.4H2O、0.17g ZnCl2Be dissolved in 40mL ethylene glycol and
In the dicyandiamide solution of diglycol, magnetic agitation 30min, forms orange-yellow uniform mixed liquor at room temperature.By the poly- of 1g
Aziridine (PEI), 3.6g anhydrous sodium acetate are added in the mixed liquor stirred evenly, magnetic agitation about 30min, then to mixed
Close the ultrasonic treatment that liquid carries out about 10min.Mixed liquor is moved in the reaction kettle of the polytetrafluoroethyllining lining of 100ml and is sealed.
Reaction kettle is put into baking oven, in 200 DEG C of reaction 12h.After reaction kettle is cooling, with alcohol and deionized water wash products 4-5
It is secondary, then in a vacuum drying oven 70 DEG C, dry under 8h, obtain black magnetic product.
Characterization: in Fig. 2 shown in (d) and Fig. 4 (c) in ethylene glycol and diglycol dicyandiamide solution with PEI-1g
For the nano particle of coating material preparation XRD spectrum and scanning electron microscope (SEM) photograph it is found that prepared MnZn ferrite nano
Grain is spinel-type, and crystallization degree is higher, and crystal form is good；Minimum nanoparticle agglomerates form the big nanometer of uniform-spherical
Particle.It is calculated through nanomeasure particle diameter distribution software statistics, average grain diameter is about 230nm, the standard deviation of particle diameter distribution
Poor smaller, morphological rules, good dispersion.
Embodiment 5
Weigh 1.35g FeCl3.6H2O、0.247g MnCl2.4H2O、0.17g ZnCl2Be dissolved in 40mL ethylene glycol and
In the dicyandiamide solution of diglycol, magnetic agitation 30min, forms orange-yellow uniform mixed liquor at room temperature.By the poly- of 1g
Vinylpyrrolidone (PVP), 3.6g anhydrous sodium acetate are added in the mixed liquor stirred evenly, magnetic agitation about 30min, then
The ultrasonic treatment of about 10min is carried out to mixed liquor.Mixed liquor is moved to close in the reaction kettle of the polytetrafluoroethyllining lining of 100ml
Envelope.Reaction kettle is put into baking oven, in 200 DEG C of reaction 12h.After reaction kettle is cooling, with alcohol and deionized water wash products
4-5 times, then in a vacuum drying oven 70 DEG C, dry under 8h, obtain black magnetic product.
Characterization: in Fig. 2 shown in (e) and Fig. 4 (d) in ethylene glycol and diglycol dicyandiamide solution with PVP-1g
For the nano particle of coating material preparation XRD spectrum and scanning electron microscope (SEM) photograph it is found that prepared MnZn ferrite nano
Grain is spinel-type, and crystallization degree is higher, and crystal form is good；Minimum nanoparticle agglomerates form the big nanometer of uniform-spherical
Particle.It is calculated through nanomeasure particle diameter distribution software statistics, average grain diameter is about 280nm, and particle diameter distribution is uniform, shape
Looks rule, good dispersion.
Embodiment 6
Weigh 1.35g FeCl3.6H2O、0.247g MnCl2.4H2O、0.17g ZnCl2Be dissolved in 40mL ethylene glycol and
In the dicyandiamide solution of diglycol, magnetic agitation 30min, forms orange-yellow uniform mixed liquor at room temperature.By 0.5g's
Polyethylene glycol (PEG), the 3.6g anhydrous sodium acetate of polyethyleneimine (PEI) and 0.5g are added in the mixed liquor stirred evenly,
Magnetic agitation about 30min, then the ultrasonic treatment of about 10min is carried out to mixed liquor.Mixed liquor is moved to the polytetrafluoro of 100ml
It is sealed in the reaction kettle of ethylene liner.Reaction kettle is put into baking oven, in 200 DEG C of reaction 12h.After reaction kettle is cooling, wine is used
Essence and deionized water wash products 4-5 times, then in a vacuum drying oven 70 DEG C, dry under 8h, obtain black magnetic product.
Embodiment 7
Weigh 1.35g FeCl3.6H2O、0.247g MnCl2.4H2O、0.17g ZnCl2Be dissolved in 40mL ethylene glycol and
In the dicyandiamide solution of diglycol, magnetic agitation 30min, forms orange-yellow uniform mixed liquor at room temperature.By 0.5g's
Polyethylene glycol (PEG), the 3.6g anhydrous sodium acetate of polyvinylpyrrolidone (PVP) and 0.5g are added to the mixed liquor stirred evenly
In, magnetic agitation about 30min, then the ultrasonic treatment of about 10min is carried out to mixed liquor.Mixed liquor is moved into the poly- of 100ml
It is sealed in the reaction kettle of tetrafluoroethene liner.Reaction kettle is put into baking oven, in 200 DEG C of reaction 12h.After reaction kettle is cooling,
With alcohol and deionized water wash products 4-5 times, then in a vacuum drying oven 70 DEG C, dry under 8h, obtain black magnetic production
Object.
Characterization: in Fig. 2 shown in (f) and Fig. 4 (e) in ethylene glycol and diglycol dicyandiamide solution with PEG/
The XRD spectrum and scanning electron microscope (SEM) photograph that PVP-0.5g/0.5g is the nano particle of coating material preparation are it is found that prepared MnZn
Ferrite nanometer particle is spinel-type, and crystallization degree is higher, and crystal form is good；Minimum nanoparticle agglomerates form uniform ball
The big nano particle of shape.It is calculated through nanomeasure particle diameter distribution software statistics, average grain diameter is about 330nm, partial size
It is distributed uniform, morphological rules, good dispersion.
Conclusion
XRD spectrum show different dicyandiamide solutions and variety classes based on ethylene glycol, dosage coating material not
The crystal phase that will affect target product is spinel-type magnetic iron ore phase MnZn ferrite nanometer particle (Fig. 1, Fig. 2).
It can be seen that it can by using different different dicyandiamide solutions based on ethylene glycol and not from scanning electron microscope (SEM) photograph
Same type, dosage coating material regulate and control the size of MnZn ferrite magnetic nano particle, this invention successfully realizes
Average grain diameter is regulated and controled at 30-350nm range (Fig. 4).
The specific embodiment of the application above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
The limitation to the application protection scope therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, under the premise of not departing from technical scheme design, various modifications and improvements can be made, these belong to this
The protection scope of application.
Claims (7)
1. the preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size, which comprises the steps of:
(1) preparation of precursor liquid is reacted:
Fe will be contained respectively3+、Mn2+、Zn2+Salt be dissolved in the dicyandiamide solution based on ethylene glycol, magnetic agitation at room temperature, shape
At orange-yellow uniform mixed liquor；
(2) generation of spherical shape MnZn ferrite magnetic nano particle:
Coating material, sodium acetate are added in the mixed liquor that step (1) obtains, then magnetic agitation is ultrasonically treated, surpass
It is transferred in reaction kettle and seals after sonication, reaction kettle is heated at 160-200 DEG C, react 12-20h；
(3) post-processing of product:
After reaction kettle is cooling, then wash products are dried in a vacuum drying oven, obtain black magnetic product；
The dicyandiamide solution based on ethylene glycol is ethylene glycol and tetraethylene-glycol, ethylene glycol and diglycol, second
One of two alcohol and waters；
The coating material is one of polyethylene glycol (PEG), polyvinylpyrrolidone (PVP), polyethyleneimine (PEI)
Or polyethylene glycol and polyvinylpyrrolidone mixing or polyethylene glycol and polyethyleneimine mixing；
When dicyandiamide solution is ethylene glycol and water, Mn2+When molar ratio with PEG is 7.5, prepared nano particle average grain diameter is
30nm；When dicyandiamide solution is ethylene glycol and tetraethylene-glycol, Mn2+When molar ratio with PEG is 7.5, prepared nanometer
Grain average grain diameter is 120nm；When dicyandiamide solution is ethylene glycol and diglycol, Mn2+When molar ratio with PEI is 12.5,
Prepared nano particle average grain diameter is 230nm；When dicyandiamide solution is ethylene glycol and diglycol, Mn2+With PEG and
When the molar ratio of PEI is respectively 15,25, prepared nano particle average grain diameter is 240nm；When dicyandiamide solution be ethylene glycol and
Diglycol, Mn2+When molar ratio with PVP is 12.5, prepared nano particle average grain diameter is 280nm；Work as solvent
System is ethylene glycol and diglycol, Mn2+When being respectively 15,25 with the molar ratio of PEG and PVP, prepared nanometer
Grain average grain diameter is 330nm；When dicyandiamide solution is ethylene glycol and diglycol, Mn2+When molar ratio with PEG is 7.5, institute
The nano particle average grain diameter of preparation is 350nm.
2. the preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size according to claim 1, special
Sign is, Fe3+、Mn2+、Zn2+, sodium acetate molar ratio be 0.5:0.5:2:8.
3. the preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size according to claim 1, special
Sign is, polyethylene glycol in step (2), polyvinylpyrrolidone, polyethyleneimine relative molecular mass be respectively 6000,
10000,10000, Mn2+Molar ratio with polyethylene glycol, polyvinylpyrrolidone, polyethyleneimine is respectively 7.5-75,12.5-
125、12.5-125。
4. the preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size according to claim 1, special
Sign is that the volume ratio of ethylene glycol and tetraethylene-glycol is 1:1-3:1, the volume ratio of ethylene glycol and diglycol
Are as follows: the volume ratio 1:1-3:1 of 1:1-3:1, ethylene glycol and water.
5. the preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size according to claim 1, special
Sign is, in step (3), the method for wash products are as follows: cleaned 4-5 times using alcohol and deionized water.
6. the preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size according to claim 1, special
Sign is, in step (3), the temperature of drying is 70 DEG C.
7. the preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size according to claim 1, special
Sign is, in step (1), Fe3+、Mn2+、Zn2+Salt be respectively FeCl3.6H2O、MnCl2.4H2O、ZnCl2。
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| CN115430443B (en) * | 2022-09-18 | 2023-07-07 | 重庆文理学院 | SrFe 12 O 19 Mxene composite catalyst, preparation method and application thereof |
| CN117838874B (en) * | 2024-03-07 | 2024-06-11 | 山东第一医科大学(山东省医学科学院) | Preparation method and application of gadolinium-platinum radiotherapy sensitizer |
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