CN110436529A - A kind of Fe can be used for magnetic thermotherapy3O4The preparation method of nano-bar material - Google Patents
A kind of Fe can be used for magnetic thermotherapy3O4The preparation method of nano-bar material Download PDFInfo
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- CN110436529A CN110436529A CN201910845321.4A CN201910845321A CN110436529A CN 110436529 A CN110436529 A CN 110436529A CN 201910845321 A CN201910845321 A CN 201910845321A CN 110436529 A CN110436529 A CN 110436529A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P2006/32—Thermal properties
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Abstract
The invention discloses a kind of Fe that can be applied to magnetic thermotherapeutic agent3O4The preparation method of nano-bar material, this method is including the use of FeCl3·6H2O is raw material, synthesizes the Fe with nanorod shape with high annealing method by hydro-thermal reaction3O4Magnetic material.Experimental implementation of the invention is easy, and uncontrollable factor is less, can be prepared on a large scale in general environment.Prepared by the method Fe3O4Nano-bar material has good magnetic heating performance, can satisfy the research and development in medicine for the magnetic thermotherapeutic agent of tumour, to increase magnetic thermotherapy effect.
Description
Technical field
The invention belongs to the biomedical applications field of nano material, and in particular to a kind of magnetic thermotherapeutic agent that can be applied to
Fe3O4The preparation method of nano-bar material.
Background technique
In recent years, as the technology of preparing of magnetic Nano material is constantly mature, type is gradually enriched, the research of this material
Field is also extending therewith.In addition to conventional electronics device research and development arrive magnetic memory device application, magnetic Nano material due to
With good biological safety, surface modificability, special vivo performance and unique magnetic performance, at present in biological section
Technology, multiple research fields such as biomedicine all relate to, and show considerable application prospect.Including as high property
It can magnetic thermotherapeutic agent treatment malignant tumour.Bio-medical magnetic Nano material carrying medicament is utilized, is directed by externally-applied magnetic field
It is delivered at target cell, recycles magnetothermal effect, be allowed to generate heat under alternating magnetic field, achieve the purpose that targeted therapy.By
It is not influenced by chemical reagent in the movement of magnetic Nano material in vivo, therefore may be applied to medicine contrast imaging,
New selection and hope are provided for the diagnosing and treating of infantile tumour.
Although the bio-medical magnetic Nano material developed at present has many good qualities, most as magnetic thermotherapeutic agent
Big difficulty and challenge is high-cost synthesis technology and weak thermal conversion efficiency, such as Fe3O4Nano particle, Fe3O4Nanosphere and
Various iron-based oxide-based nanomaterials, as the 9nm Fe mentioned in patent 201510071614.33O4Nano particle is as magnetic warm
The application for treating agent reaches (42 DEG C) of magnetic thermotherapy required temperature in the magnetic field of 500Oe and needs the relatively long time, to influence it
Service performance.Controllable bio-medical Fe3O4The application of nano-bar material is also more and more extensive, has developed many preparation sides so far
Method, such as the synthesis of coprecipitation, sol-gel synthesis method, hydro-thermal reaction, phonochemical reaction, laser pyrolysis processes, micro emulsion method.In
In these methods, traditional method is thermal decomposition molysite, but needs to react at high temperature, for example decomposes iron oleate required temperature height
Up to 200 DEG C, so consumed energy is higher in industrialization production, condition is harsher, and at high cost and yield is relatively low.In order to big
Scale industrialization prepares Fe3O4Nano material, and low cost, feasible effective synthesis technology and application value, hydro-thermal are considered simultaneously
Synthetic method is preparing bio-medical Fe3O4Become preferred option when nano material, and passes through adjusting hydrothermal reaction time or reactant
Concentration can effectively controlled material size and size, to effectively promote the magnetic heating performance of material.In addition, nano-bar material
Due to its adjustable draw ratio and strong anisotropy, so that it, which has, is easy to the magnetic performance of other shapes material, and Fe3O4
There is presently no corresponding document reports for the magnetic heating performance of nano-bar material.Therefore, bio-medical Fe is prepared using hydro-thermal method3O4
Nano-bar material simultaneously studies its magnetic heating performance, to realize the development of high-performance magnetism thermotherapeutic agent and its practicing clinical application in magnetic thermotherapy
Provide good Research foundation.
Summary of the invention
The technical problem to be solved by the present invention is in the prior art the shortcomings that, how to select appropriate predecessor with
And experiment condition, prepare the medical Fe of the higher object of heat production specific power (SAR) value3O4Nano-bar material, can be in magnetic thermotherapy
It is applied in the research and development of agent.
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide a kind of Fe that can be applied to magnetic thermotherapeutic agent3O4It receives
The preparation method of rice bar material, this method are to utilize FeCl3·6H2O is raw material, and predecessor β-is made by hydrothermal synthesis method
Then predecessor β-FeOOH and trioctylamine and elaidin reaction are obtained colloidal mixture by FeOOH, finally use high annealing method
Prepare monodispersed Fe3O4Nano-bar material.
Preferably, described method includes following steps:
(1) by the FeCl of 0.15mol/L3·6H2O solution carries out hydro-thermal reaction 2- at 100-105 DEG C of autoclave
3h, the yellow mercury oxide that natural cooling obtains are respectively washed with deionized water and alcohol, and are dried under the conditions of 60 DEG C, and β-is obtained
FeOOH presoma；
(2) it weighs the β-FeOOH presoma that step (1) obtains to evenly spread in trioctylamine by ultrasound 2-3h, and adds
Enter oleic acid stirring 1-2h, obtains colloidal mixture after being centrifuged 5-15min under the conditions of 7500-8500rpm, wherein β-FeOOH exists
The mass fraction dispersed in trioctylamine is 3.33g/L, and the volume ratio that oleic acid and trioctylamine is added is 30:1；
(3) colloidal mixture obtained in step (2) is transferred to high temperature process furnances and carries out reduction process, completed wait react
Natural cooling obtains black powder Fe afterwards3O4Nano-bar material.
Preferably, the atmosphere used when natural cooling in the step (3) is Ar and H2Mixed atmosphere, volume ratio are
15-19:1, total throughput are 80-100 ml/min (SCCM).
Preferably, the heating rate in the step (3) when natural cooling is 5-10 DEG C/min, and annealing temperature is 340 DEG C.
Another object of the present invention is to provide a kind of Fe applied to magnetic thermotherapeutic agent3O4The preparation method of nano-bar material
The Fe prepared3O4Nano-bar material, containing Fe described in 0.2mg/mL3O4The aqueous dispersion of nano-bar material is in 10min
Heat production reach 42 DEG C, heat production specific power SAR value reaches 1045W/g.
Another object of the present invention is to provide a kind of Fe applied to magnetic thermotherapeutic agent3O4The preparation method of nano-bar material
The Fe prepared3O4Nano-bar material is in the Fe for preparing the application in magnetic thermotherapeutic agent3O4The application of nano-bar material.
The present invention has the following characteristics that compared with existing technology
1. the Fe of this method preparation3O4Nano material has club shaped structure, and draw ratio can regulate and control.It is of the invention simultaneously
Experimental implementation is easy, and uncontrollable factor is less, can be prepared on a large scale in general environment.
2. the Fe of this method preparation3O4The magnetic heating performance of nano-bar material is significant to increase relative to traditional magnetic Nano material
By force.The length of preparation is 370nm, and diameter is the Fe of 80nm3O4Nanometer rods (the hydro-thermal time for preparing predecessor FeOOH is 6h) point
Aproll solution, when concentration is 0.2mg/mL, it is only necessary to which 10min can reach 42 DEG C, that is, be suitble to the application of high-temp magnetic heat.When its concentration
When continuing to increase to 0.4mg/mL, the rate of heat addition is obviously increased.It is corresponding, the Fe of 0.2mg/mL concentration3O4Nanometer rods are in lower magnetic
(308Oe) has maximum SAR value 1045W/g off field, further demonstrates that its good magnetic heating performance, is the research and development of magnetic thermotherapeutic agent
With the basis strong using offer.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.
Fig. 1: the Fe prepared in embodiment 1-33O4The X ray diffracting spectrum of nanometer rods.
Fig. 2: the Fe prepared in embodiment 1-33O4The scanning electron microscope image of nanometer rods, wherein a is Fe3O4- 4h, b are
Fe3O4-10h；C is Fe3O4-6h。
Fig. 3: Fe in embodiment 33O4The images of transmissive electron microscope and element distribution image of -6h；Wherein Fig. 3 a is Fe3O4- 6h's
Images of transmissive electron microscope, Fig. 3 b are Fe3O4The high-resolution-ration transmission electric-lens image and element distribution image of -6h.
Fig. 4: Fe in embodiment 33O4The fine spectrogram picture of the x-ray photoelectron of -6h；Wherein Fig. 4 a is Fe in embodiment 33O4-
The fine spectrogram picture of the x-ray photoelectron of the Fe 2p of 6h, Fig. 4 b are Fe in embodiment 33O4The x-ray photoelectron of the O1s of -6h is fine
Spectrogram picture.
Fig. 5: Fe in embodiment 1-33O4The hysteresis loop of nanometer rods；
Fig. 6: various concentration Fe in embodiment 33O4The rate of heat addition performance image of -6h sample.
Fig. 7: various concentration Fe in embodiment 33O4The SAR of -6h sample.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings.It is hereby stated that embodiments set forth herein is only
For the description of the invention and explanation, limitation is not constituted to the present invention.
Embodiment 1
Weigh 1.6g FeCl3·6H2O is simultaneously dissolved in 60mL deionized water, and prepared solution is transferred to appearance
It is sealed in the high-pressure hydrothermal reaction kettle that product is 100mL.Reaction kettle is then placed in hydro-thermal reaction in the baking oven that temperature is 100 DEG C
4h, cooled to room temperature.Then experiment gained yellow mercury oxide deionized water and alcohol are respectively washed 3 times, centrifugation is simultaneously
It is dried under the conditions of 60 DEG C, obtains yellow powder β-FeOOH, it is named as FeOOH-4h by us herein.Then, 20mg is weighed
β-FeOOH powder, places them into 6mL trioctylamine, and ultrasound 2h, keeps it evenly dispersed in trioctylamine in ultrasonic cleaning machine.
200 μ L oleic acid are added in the suspension obtained after distribution, 1h are sufficiently stirred, then obtained mixture is transferred to centrifuge,
Colloidal mixture is obtained after being centrifuged 5min at 7500rpm.The above mixture is transferred to the high temperature process furnances of sealing, in boiler tube
In be passed through Ar/H2Mixed atmosphere (wherein Ar throughput 75SCCM；H2Flow 5SCCM).With the speed of 5 DEG C/min under the atmosphere
Tube furnace is warming up to 340 DEG C by rate, is made its cooled to room temperature after keeping the temperature 2h, is obtained black powder.It will be obtained with n-hexane
Black powder clean 3 times, under the conditions of 60 DEG C dry after Fe can be obtained3O4The sample of nanometer rods.It is named as Fe3O4-4h。
We are to the Fe obtained in embodiment 13O4The test and analysis of X ray diffracting spectrum are carried out, as a result such as attached drawing 1
It is shown.By being compared with standard peak position, it can be seen that the sample obtained in embodiment 1 is the Fe of pure phase3O4.Attached drawing 2a is
Fe3O4The scanning electron microscopic picture of -4h, where it can be seen that sample shows the shape of nanometer rods, average length about~460nm,
Diameter about~80nm.Attached drawing 5 gives Fe3O4The hysteresis loop of -4h, saturation magnetization are about 68emu/g.
Embodiment 2
Weigh 1.6g FeCl3·6H2O is simultaneously dissolved in 60mL deionized water, and prepared solution is transferred to appearance
It is sealed in the high-pressure hydrothermal reaction kettle that product is 100mL.Then reaction kettle is placed in the baking oven that temperature is 100 DEG C and keeps the temperature 10h, from
So it is cooled to room temperature.Then experiment gained yellow mercury oxide deionized water and alcohol are respectively washed 3 times, are centrifuged and at 80 DEG C
Under the conditions of dry, obtain yellow powder β-FeOOH, it is named as FeOOH-10h by us herein.Then, 20mg β-is weighed
FeOOH powder places them into 6mL trioctylamine, and ultrasound 2h, keeps it evenly dispersed in trioctylamine in ultrasonic cleaning machine.In
200 μ L oleic acid are added in the suspension obtained after dispersion, 2h are sufficiently stirred, then obtained mixture is transferred to centrifuge, In
Colloidal mixture is obtained after being centrifuged 15min under 7500rpm.The above mixture is transferred to the high temperature process furnances of sealing, in boiler tube
In be passed through Ar/H2Mixed atmosphere (wherein Ar throughput 75SCCM；H2Flow 5SCCM).With the speed of 10 DEG C/min under the atmosphere
Tube furnace is warming up to 340 DEG C by rate, is made its cooled to room temperature after keeping the temperature 5h, is obtained black powder.It will be obtained with n-hexane
Black powder clean 3 times, under the conditions of 80 DEG C dry after Fe can be obtained3O4The sample of nanometer rods, is named as Fe3O4-10h。
We are to the Fe obtained in embodiment 23O4The test and analysis of X ray diffracting spectrum are carried out, as a result such as attached drawing 1
It is shown.By being compared with standard peak position, it can be seen that the sample obtained in embodiment 2 is the Fe of pure phase3O4.Attached drawing 2b is
Fe3O4The scanning electron microscopic picture of -10h, where it can be seen that sample shows the shape of nanometer rods, average length about~
252nm, diameter about~101nm.Attached drawing 5 gives Fe3O4The hysteresis loop of -10h, saturation magnetization are about 75emu/g.
Embodiment 3
Weigh 1.6g FeCl3·6H2O is simultaneously dissolved in 60mL deionized water, and prepared solution is transferred to appearance
It is sealed in the high-pressure hydrothermal reaction kettle that product is 100mL.Then reaction kettle is placed in the baking oven that temperature is 100 DEG C and keeps the temperature 6h, from
So it is cooled to room temperature.Then experiment gained yellow mercury oxide deionized water and alcohol are respectively washed 5 times, are centrifuged and at 60 DEG C
Under the conditions of dry, obtain yellow powder β-FeOOH, it is named as FeOOH-6h by us herein.Then, 20mg β-is weighed
FeOOH powder places them into 6mL trioctylamine, and ultrasound 3h, keeps it evenly dispersed in trioctylamine in ultrasonic cleaning machine.In
200 μ L oleic acid are added in the suspension obtained after dispersion, 1h are sufficiently stirred, then obtained mixture is transferred to centrifuge, In
Colloidal mixture is obtained after being centrifuged 5min under 8500rpm.The above mixture is transferred to the high temperature process furnances of sealing, in boiler tube
It is passed through Ar/H2Mixed atmosphere (wherein Ar throughput 95SCCM；H2Flow 5SCCM).With the rate of 5 DEG C/min under the atmosphere
Tube furnace is warming up to 340 DEG C, makes its cooled to room temperature after keeping the temperature 2h, obtains black powder.It will be obtained with n-hexane
Black powder cleans 5 times, and Fe can be obtained after drying under the conditions of 60 DEG C3O4The sample of nanometer rods, is named as Fe3O4-6h。
We are to the predecessor FeOOH-6h and Fe obtained in embodiment 33O4- 6h has carried out the test of X ray diffracting spectrum
And analysis, as a result as shown in Fig. 1.By being compared with standard peak position, it can be seen that obtaining sample in embodiment 3 is pure phase
Fe3O4.Attached drawing 2c is Fe3O4The scanning electron microscopic picture of -6h is averaged where it can be seen that sample shows the shape of nanometer rods
Length about~370nm, diameter about~80nm.Attached drawing 3a gives Fe3O4The images of transmissive electron microscope of -6h nanometer rods, it is observed to receive
The pattern of rice stick is identical as scanning electron microscope.Attached drawing 3b is Fe3O4The high-resolution-ration transmission electric-lens image and distribution diagram of element of nanometer rods
Picture, therefrom it can be seen that Fe3O4Lattice structure be evenly distributed on Fe, O element of sample interior.Attached drawing 4a, 4b are provided respectively
Fe3O4The fine x-ray photoelectron spectroscopy figure of Fe 2p and O1s in -6h sample.Attached drawing 5 gives Fe3O4The magnetic hysteresis of -6h is returned
Line, saturation magnetization are about 70emu/g.
Next, by Fe obtained in embodiment 33O4- 6h sample is placed in alternating magnetic field (setting according to various concentration
Magnetic field size is 308Oe, alternative frequency 360kHz) carry out external elevated temperature test.Three kinds of various concentrations are chosen in this experiment
Fe3O4Nanorods Samples: 0.1mg/mL, 0.2mg/mL and 0.4mg/mL, heating curve are as shown in Fig. 6.It can be seen that dense
Degree needs 10min that can reach 42 DEG C when being 0.2mg/mL, and the sample of 0.4mg/mL has most fast heating rate, and short
42 DEG C can be reached in 6min, that is, be suitble to the application of high-temp magnetic heat.According to the initial slope of heating curve, attached drawing 7 is calculated
Fe3O4The specific absorption rate of -6h nanometer rods various concentration, therefrom it can be seen that concentration is the specific absorption rate height of the sample of 0.2mg/mL
Up to 1045W/g, the sample is characterized when concentration is 0.2mg/mL with best magnetic heating performance, is expected to be applied to high-performance magnetism heat
Treat the research and development of agent.
Claims (6)
1. a kind of Fe that can be applied to magnetic thermotherapeutic agent3O4The preparation method of nano-bar material, it is characterised in that: this method is to utilize
FeCl3·6H2O is raw material, predecessor β-FeOOH is made by hydrothermal synthesis method, then by predecessor β-FeOOH and trioctylamine
Colloidal mixture is obtained with elaidin reaction, monodispersed Fe is finally prepared using high annealing method3O4Nano-bar material.
2. preparation method according to claim 1, it is characterised in that include the following steps:
(1) by the FeCl of 0.15mol/L3·6H2O solution carries out hydro-thermal reaction 4-10h at 100-105 DEG C of autoclave, from
So cooling obtained yellow mercury oxide is respectively washed with deionized water and alcohol, and is dried under the conditions of 60-80 DEG C, and β-is obtained
FeOOH presoma；
(2) it weighs the β-FeOOH presoma that step (1) obtains to evenly spread in trioctylamine by ultrasound 2-3h, and oil is added
Acid stirring 1-2h, obtains colloidal mixture after being centrifuged 5-15min under the conditions of 7500-8500rpm, wherein β-FeOOH is pungent three
The mass fraction dispersed in amine is 3.33g/L, and the volume ratio that oleic acid and trioctylamine is added is 30:1；
(3) by colloidal mixture obtained in step (2) be transferred to high temperature process furnances carry out reduction process, to after the reaction was completed from
So cooling obtains black powder Fe3O4Nano-bar material.
3. preparation method according to claim 2, it is characterised in that: the gas used when natural cooling in the step (3)
Atmosphere is Ar and H2Mixed atmosphere, volume ratio 15-19:1, total throughput are 80-100 ml/min.
4. preparation method according to claim 2, it is characterised in that: the heating speed in the step (3) when natural cooling
Rate is 5-10 DEG C/min, and annealing temperature is 340 DEG C.
5. the Fe prepared according to preparation method described in any of the above-described claim3O4Nano-bar material, it is characterised in that:
Containing Fe described in 0.2mg/mL3O4Heat production of the aqueous dispersion of nano-bar material in 10min reaches 42 DEG C, heat production specific power
SAR value reaches 1045W/g.
6. Fe as claimed in claim 53O4Nano-bar material is preparing the application in magnetic thermotherapeutic agent.
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