CN110436529B - Fe for magnetic thermal therapy3O4Preparation method of nano rod material - Google Patents
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Abstract
The inventionDiscloses Fe which can be applied to magnetic thermal therapy agent3O4A method for preparing a nanorod material, the method comprising using FeCl3·6H2O is used as a raw material, and Fe with a nanorod shape is synthesized by a hydrothermal reaction and high-temperature annealing method3O4A magnetic material. The method has the advantages of simple and convenient experimental operation and few uncontrollable factors, and can be used for large-scale preparation in a universal environment. Fe prepared by the invention3O4The nano rod material has good magnetic thermal property, and can meet the research and development of a magnetic thermal therapeutic agent for tumors in medicine, so that the magnetic thermal curative effect is increased.
Description
Technical Field
The invention belongs to the field of biomedical application of nano materials, and particularly relates to Fe capable of being applied to a magnetic thermal therapy agent3O4A method for preparing a nano rod material.
Background
In recent years, as the preparation technology of magnetic nano materials is mature and the types of the materials are gradually enriched, the research field of the materials is expanded. Except for the application of the traditional electronic device in the development of a magnetic memory device, the magnetic nano material has good biological safety, surface modifiability, special in-vivo performance and unique magnetic performance, is related in a plurality of research fields of bioscience technology, biomedicine and the like at present, and shows considerable application prospect. Including as a high performance magnetic hyperthermia agent for the treatment of malignant tumors. The biomedical magnetic nano material is used for loading the medicine, the medicine is directionally conveyed to a target cell through an external magnetic field, and then the heat is generated under an alternating magnetic field by using the magnetocaloric effect, so that the aim of targeted therapy is fulfilled. The magnetic nano material can be applied to medical contrast imaging because the motion of the magnetic nano material in the body is not influenced by chemical agents, and provides new choices and hopes for the diagnosis and treatment of early tumors.
Although biomedical magnetic nanomaterials have been developed to date with many advantages, the greatest difficulties and challenges as hyperthermia agents are the high cost of the synthesis process and the poor heat transfer efficiency, such as Fe3O4Nanoparticles of Fe3O4Nanospheres and various iron-based oxide nanomaterials, such as 9nm Fe mentioned in patent 201510071614.33O4The application of the nano particles as the magnetic thermal therapy agent requires a relatively long time to reach the temperature (42 ℃) required by the magnetic thermal therapy in the magnetic field of 500Oe, thereby influencing the use performance of the nano particles. Adjustable biomedical Fe3O4The application of the nano rod material is more and more extensive, and a plurality of preparation methods such as coprecipitation method, sol-gel synthesis method, hydrothermal reaction, phonochemical reaction, laser pyrolysis method and microemulsion method are developed up to now. Among these methods, the conventional method is to thermally decompose iron salt, but the reaction at high temperature is required, for example, the temperature required for decomposing iron oleate is as high as 200 ℃, so the energy consumption in industrial production is higher, the conditions are more severe, the cost is high and the yield is lower. For large-scale industrial preparation of Fe3O4Nano material, low cost, feasible and effective synthesis process and application value are considered, and the hydrothermal synthesis method is used for preparing biomedical Fe3O4The nano material becomes the preferred scheme, and the size and the dimension of the material can be effectively regulated and controlled by regulating and controlling the hydrothermal reaction time or the concentration of reactants, so that the magnetocaloric performance of the material is effectively improved. In addition, the nanorod material has magnetic properties easy for materials with other shapes due to the adjustable length-diameter ratio and strong anisotropy, while Fe3O4The magnetocaloric properties of the nanorod materials are not reported in corresponding documents at present. Thus, hydrothermal method is used to prepare biomedical Fe3O4The nano rod material and the research on the magnetic thermal performance thereof provide a good research foundation for the research and the application of the high-performance magnetic thermal therapy agent in the practice clinical application of the magnetic thermal therapy.
Disclosure of Invention
The technical problem to be solved by the invention is how to select proper precursors and experimental conditions to prepare medical Fe with high specific power of specific heat production (SAR) value aiming at the defects in the prior art3O4Nanorod materials, enabling their use in the development of magnetic hyperthermia agents.
In order to solve the above technical problems, it is an object of the present invention to provide Fe applicable to a magnetic thermal therapeutic agent3O4The preparation method of the nano rod material utilizes FeCl3·6H2O is taken as a raw material, a precursor beta-FeOOH is prepared by a hydrothermal synthesis method, then the precursor beta-FeOOH is reacted with trioctylamine and oleic acid to obtain a colloidal mixture, and finally, a high-temperature annealing method is adopted to prepare monodisperse Fe3O4A nanorod material.
Preferably, the method comprises the steps of:
(1) FeCl of 0.15mol/L3·6H2Performing hydrothermal reaction on the O solution for 2-3h at the temperature of high-pressure reaction kettle of 100 ℃ -;
(2) weighing the beta-FeOOH precursor obtained in the step (1), uniformly dispersing the beta-FeOOH precursor into trioctylamine by ultrasonic for 2-3h, adding oleic acid, stirring for 1-2h, and centrifuging for 5-15min under the condition of 7500 plus 8500rpm to obtain a colloidal mixture, wherein the mass fraction of the beta-FeOOH dispersed in the trioctylamine is 3.33g/L, and the volume ratio of the added oleic acid to the trioctylamine is 30: 1;
(3) transferring the colloidal mixture obtained in the step (2) to a high-temperature tube furnace for reduction, and naturally cooling to obtain black powder Fe after the reaction is finished3O4A nanorod material.
Preferably, the atmosphere used in the natural cooling in the step (3) is Ar and H2Mixed atmosphere with volume ratio of 15-19:1 and total gas flow of 80-100 ml/min (SCCM).
Preferably, the heating rate of the natural cooling in the step (3) is 5-10 ℃/min, and the annealing temperature is 340 ℃.
Another object of the present invention is to provide Fe for magnetic thermal therapeutic agent3O4Fe prepared by preparation method of nanorod material3O4Nanorod material containing 0.2mg/mL of said Fe3O4The heat generation of the aqueous dispersion of the nano rod material reaches 42 ℃ within 10min, and the SAR value of the heat generation specific power reaches 1045W/g.
Another object of the present invention is to provide Fe for magnetic thermal therapeutic agent3O4Fe prepared by preparation method of nanorod material3O4Fe of nano-rod material in application of preparing magnetic thermal therapy agent3O4Application of nano rod material.
Compared with the prior art, the invention has the following characteristics:
1. fe prepared by the method3O4The nanometer material has a rod-shaped structure, and the length-diameter ratio of the nanometer material can be regulated and controlled. Meanwhile, the method is simple and convenient in experimental operation, has few uncontrollable factors, and can be used for large-scale preparation in a universal environment.
2. Fe prepared by the method3O4The magnetocaloric performance of the nano rod material is obviously enhanced compared with that of the traditional magnetic nano material. Prepared Fe with the length of 370nm and the diameter of 80nm3O4When the concentration of the nano rod (the hydrothermal time for preparing precursor FeOOH is 6h) dispersed aqueous solution is 0.2mg/mL, the temperature can reach 42 ℃ only within 10min, and the nano rod is suitable for high-temperature magnetocaloric application. As its concentration continued to increase to 0.4mg/mL, the heating rate increased significantly. Corresponding, 0.2mg/mL concentration of Fe3O4The nanorods have the maximum SAR value of 1045W/g under a lower magnetic field (308Oe), further indicating good magnetocaloric properties, and providing a powerful basis for the development and utilization of magnetocaloric therapeutics.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
FIG. 1: fe prepared in examples 1 to 33O4The X-ray diffraction pattern of the nano-rod.
FIG. 2: fe prepared in examples 1 to 33O4Scanning electron microscope image of the nanorods, wherein a is Fe3O4-4h, b is Fe3O4-10 h; c is Fe3O4-6h。
FIG. 3: fe in example 33O4-a transmission electron microscope image and an elemental distribution image of 6 h; wherein FIG. 3a is Fe3O4Transmission electron microscopy image of-6 h, FIG. 3b is Fe3O4-6h high resolution transmission electron microscopy images and elementsA pixel distribution image.
FIG. 4: fe in example 33O4-6h of an X-ray photoelectron fine spectrum image; wherein FIG. 4a is Fe in example 33O4X-ray photoelectron spectroscopy image of Fe 2p at-6 h, FIG. 4b is Fe in example 33 O 46h of an X-ray photoelectron fine spectrum image of O1 s.
FIG. 5: fe in examples 1 to 33O4A hysteresis loop of the nanorod;
FIG. 6: different concentrations of Fe in example 33O4Heating rate performance image of 6h sample.
FIG. 7: different concentrations of Fe in example 33O4SAR for 6h samples.
Detailed Description
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It is to be understood that the examples set forth herein are for the purpose of illustration and explanation only and are not intended as a definition of the limits of the invention.
Example 1
Weigh 1.6g FeCl3·6H2And O is dissolved in 60mL of deionized water, and the prepared solution is transferred to a high-pressure hydrothermal reaction kettle with the volume of 100mL and sealed. And then placing the reaction kettle in an oven with the temperature of 100 ℃ for hydrothermal reaction for 4h, and naturally cooling to room temperature. The yellow precipitate from the experiment was then washed 3 times with deionized water and alcohol, respectively, centrifuged and dried at 60 ℃ to give a yellow powder β -FeOOH, which we named here as FeOOH-4 h. Subsequently, 20mg of β -FeOOH powder was weighed, put into 6mL of trioctylamine, and sonicated in a sonicator for 2h to uniformly disperse in trioctylamine. To the suspension obtained after dispersion, 200. mu.L of oleic acid was added, and the mixture was stirred well for 1 hour, and then the resulting mixture was transferred to a centrifuge and centrifuged at 7500rpm for 5 minutes to obtain a gel-like mixture. Transferring the mixture to a sealed high-temperature tube furnace, and introducing Ar/H into the tube furnace2Mixed atmosphere of (wherein the Ar gas flow is 75 SCCM; H)2Flow 5 SCCM). Heating the tube furnace to 340 ℃ at the speed of 5 ℃/min under the atmosphere, preserving heat for 2h, and naturally cooling to room temperature to obtain the productBlack powder. Washing the obtained black powder with n-hexane for 3 times, and oven drying at 60 deg.C to obtain Fe3O4A sample of nanorods. Is named as Fe3O4-4h。
We performed on the Fe obtained in example 13O4The X-ray diffraction patterns were tested and analyzed, and the results are shown in fig. 1. By comparison with the standard peak positions, it can be seen that the sample obtained in example 1 is phase-pure Fe3O4. FIG. 2a is Fe3O4-4h of scanning electron microscopy, wherein the sample can be seen to take the shape of nanorods, with an average length of about-460 nm and a diameter of about-80 nm. FIG. 5 shows Fe3O4A hysteresis loop of 4h with a saturation magnetization of about 68 emu/g.
Example 2
Weigh 1.6g FeCl3·6H2And O is dissolved in 60mL of deionized water, and the prepared solution is transferred to a high-pressure hydrothermal reaction kettle with the volume of 100mL and sealed. And then placing the reaction kettle in an oven with the temperature of 100 ℃ for heat preservation for 10 hours, and naturally cooling to room temperature. The yellow precipitate from the experiment was then washed 3 times with deionized water and alcohol, respectively, centrifuged and dried at 80 ℃ to give a yellow powder β -FeOOH, which we named here as FeOOH-10 h. Subsequently, 20mg of β -FeOOH powder was weighed, put into 6mL of trioctylamine, and sonicated in a sonicator for 2h to uniformly disperse in trioctylamine. To the suspension obtained after dispersion, 200. mu.L of oleic acid was added, stirred well for 2 hours, and the resulting mixture was transferred to a centrifuge and centrifuged at 7500rpm for 15 minutes to obtain a gelatinous mixture. Transferring the mixture to a sealed high-temperature tube furnace, and introducing Ar/H into the tube furnace2Mixed atmosphere of (wherein the Ar gas flow is 75 SCCM; H)2Flow 5 SCCM). And (3) heating the tube furnace to 340 ℃ at the speed of 10 ℃/min under the atmosphere, preserving the heat for 5h, and naturally cooling to room temperature to obtain black powder. Washing the obtained black powder with n-hexane for 3 times, and oven drying at 80 deg.C to obtain Fe3O4Nanorod sample, designated Fe3O4-10h。
We performed on the Fe obtained in example 23O4The X-ray diffraction patterns were tested and analyzed, and the results are shown in fig. 1. By comparison with the standard peak positions, it can be seen that the sample obtained in example 2 is phase-pure Fe3O4. FIG. 2b is Fe3O4Scanning electron microscopy of-10 h, wherein the sample can be seen to take the shape of nanorods, with an average length of about-252 nm and a diameter of about-101 nm. FIG. 5 shows Fe3O4A hysteresis loop of 10h, with a saturation magnetization of about 75 emu/g.
Example 3
Weigh 1.6g FeCl3·6H2And O is dissolved in 60mL of deionized water, and the prepared solution is transferred to a high-pressure hydrothermal reaction kettle with the volume of 100mL and sealed. And then placing the reaction kettle in an oven with the temperature of 100 ℃ for heat preservation for 6 hours, and naturally cooling to room temperature. The yellow precipitate from the experiment was then washed 5 times with deionized water and alcohol, respectively, centrifuged and dried at 60 ℃ to give a yellow powder β -FeOOH, which we named here as FeOOH-6 h. Subsequently, 20mg of β -FeOOH powder was weighed, put into 6mL of trioctylamine, and sonicated in a sonicator for 3 hours to uniformly disperse in trioctylamine. To the suspension obtained after dispersion, 200. mu.L of oleic acid was added, and the mixture was stirred well for 1 hour, and then the resulting mixture was transferred to a centrifuge and centrifuged at 8500rpm for 5 minutes to obtain a gel-like mixture. Transferring the mixture to a sealed high-temperature tube furnace, and introducing Ar/H into the tube furnace2Mixed atmosphere of (wherein the Ar gas flow rate is 95 SCCM; H)2Flow 5 SCCM). And (3) heating the tube furnace to 340 ℃ at the speed of 5 ℃/min under the atmosphere, preserving the heat for 2h, and naturally cooling to room temperature to obtain black powder. Washing the obtained black powder with n-hexane for 5 times, and oven drying at 60 deg.C to obtain Fe3O4Nanorod sample, designated Fe3O4-6h。
We performed on the precursors FeOOH-6h and Fe obtained in example 33O4And 6h, carrying out X-ray diffraction pattern test and analysis, and obtaining the result shown in the attached figure 1. By comparison with the standard peak position, the method canIt is seen that the sample obtained in example 3 is phase-pure Fe3O4. FIG. 2c is Fe3O4-6h, wherein the sample can be seen to take the shape of nanorods, with an average length of about 370nm and a diameter of about 80 nm. FIG. 3a shows Fe3O4And (4) a transmission electron microscope image of the nanorod for 6h, wherein the observed appearance of the nanorod is the same as that of a scanning electron microscope. FIG. 3b is Fe3O4High resolution transmission electron microscope image and element distribution image of the nano-rod, from which Fe can be seen3O4The lattice structure of the alloy and Fe and O elements which are uniformly distributed in the sample. FIGS. 4a and 4b show Fe3O4Fine X-ray photoelectron spectroscopy of Fe 2p with O1s in the 6h sample. FIG. 5 shows Fe3O4A hysteresis loop of 6h, with a saturation magnetization of about 70 emu/g.
Next, Fe obtained in example 3 was added3O4Samples were placed in alternating magnetic field (setting magnetic field size 308Oe, alternating frequency 360kHz) at different concentrations for in vitro temperature rise test for-6 h. Three different concentrations of Fe were selected in this experiment3O4Nanorod samples: 0.1mg/mL, 0.2mg/mL and 0.4mg/mL, and the temperature rise curves are shown in FIG. 6. It can be seen that the concentration of 0.2mg/mL needs 10min to reach 42 ℃, and the sample of 0.4mg/mL has the fastest heating rate and can reach 42 ℃ in as short as 6min, so that the method is suitable for high-temperature magnetocaloric application. FIG. 7 calculates Fe from the initial slope of the temperature rise curve3O4Specific absorption rates of the nanorods of-6 h in different concentrations can be seen, the specific absorption rate of a sample with the concentration of 0.2mg/mL is as high as 1045W/g, and the sample has the best magnetocaloric property when the concentration of the sample is 0.2mg/mL, so that the nanorod specific absorption rate is expected to be applied to the development of high-performance magnetic thermotherapy agents.
Claims (4)
1. Fe capable of being applied to magnetic thermal therapy agent3O4The preparation method of the nano rod material is characterized by comprising the following steps:
(1) FeCl of 0.15mol/L3·6H2The O solution is subjected to hydrothermal reaction at the temperature of 100-105 ℃ in a high-pressure reaction kettle for 4-fold reactionWashing yellow precipitates obtained by natural cooling with deionized water and alcohol respectively for 10h, and drying at the temperature of 60-80 ℃ to obtain a beta-FeOOH precursor;
(2) weighing the beta-FeOOH precursor obtained in the step (1), uniformly dispersing the beta-FeOOH precursor into trioctylamine by ultrasonic for 2-3h, adding oleic acid, stirring for 1-2h, and centrifuging for 5-15min under the condition of 7500 plus 8500rpm to obtain a colloidal mixture, wherein the mass fraction of the beta-FeOOH dispersed in the trioctylamine is 3.33g/L, and the volume ratio of the added oleic acid to the trioctylamine is 30: 1;
(3) transferring the colloidal mixture obtained in the step (2) to a high-temperature tube furnace for reduction, and naturally cooling to obtain black powder Fe after the reaction is finished3O4A nanorod material; the atmosphere used in the natural cooling is Ar and H2The volume ratio of the mixed atmosphere is 15-19:1, and the total air flow is 80-100 ml/min.
2. The method of claim 1, wherein: the heating rate in the natural cooling in the step (3) is 5-10 ℃/min, and the annealing temperature is 340 ℃.
3. Fe obtained by the production method according to any one of claims 1 to 23O4The nano rod material is characterized in that: containing 0.2mg/mL of the Fe3O4The heat generation of the aqueous dispersion of the nano rod material reaches 42 ℃ within 10min, and the SAR value of the heat generation specific power reaches 1045W/g.
4. Fe as claimed in claim 33O4The application of the nano-rod material in preparing a magnetic thermal therapy agent.
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