CN103601254A - Method for preparing gamma-Fe2O3 nano hollow sphere through laser liquid phase - Google Patents
Method for preparing gamma-Fe2O3 nano hollow sphere through laser liquid phase Download PDFInfo
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- CN103601254A CN103601254A CN201310585719.1A CN201310585719A CN103601254A CN 103601254 A CN103601254 A CN 103601254A CN 201310585719 A CN201310585719 A CN 201310585719A CN 103601254 A CN103601254 A CN 103601254A
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Abstract
The invention mainly relates to a method for preparing gamma-Fe2O3 nano hollow sphere through laser liquid phase. The method comprises the following steps: with nano-scale Fe3O4 powder as raw material, performing strong acid treatment on the raw material, magnetically separating and dispersing into a ferric nitrate solution, ultrasonically treating by using ultrasonic waves to form a mixed solution of Fe3O4 powder and uniformly dispersing the mixed solution; using pulse laser to bombard the mixed solution of Fe3O4, converging the laser beam on the surface of suspension, washing the product obtained by pulse laser bombardment respectively by using acetone and water, centrifuging, and finally drying in vacuum to obtain a required red brown sample. The process of the invention is simple, the laser effect process is safe and controllable, the problems in the existing process for preparing the gamma-Fe2O3 nano hollow sphere,that the product pollution is easily caused, the reaction condition is hard to control and high temperature and high voltage are required are overcome; and the method can be widely applied to the fields of biomagnetism separation, biosome detection, drug carrier and the like.
Description
Technical field
The invention relates to γ-Fe
2o
3the preparation method of nano-hollow ball, relates in particular to the synthetic γ-Fe of laser in liquid phase
2o
3the method of magnetic Nano hollow ball.
Background technology
Due to the widespread use of magnetic nano-particle in fields such as magnetic fluid, magnetic storage, magnetic refrigeration, absorbing material, biotechnology, catalysis and magnetic-optic devicess, its Preparation and characterization has attracted numerous investigation of materials persons' interest.Aspect biological medicine, oxidate magnetic material has better chemical stability and bio-compatibility with respect to metallicl magnetic material, thereby is widely used in magnetic bio separation, living body detection, diagnosis, treatment and the transmission of magnetic ancillary drug.
In all magnetic nano-particles, ferric oxide is as maghemite (γ-Fe
2o
3) and magnetite (Fe
3o
4) nanoparticle is because its cheap cost and good magnetic property receive much concern.Wherein, γ-Fe
2o
3due to its good thermostability and compare Fe
3o
4purposes and become study hotspot widely.Due to γ-Fe
2o
3pattern, size and dispersed practical application is had a huge impact, when nanometer scale, there is especially polymorphism, thus need a kind of can control surface pattern again can controlling dimension method synthesize.Its synthetic method has at present: the γ-Fe of 1, coprecipitation method---preparation
2o
3have water-soluble and biocompatibility, shortcoming is that the distribution of pattern and size is difficult to control, and easily generates and reunites.Referring to Jhunu C, Yousef H, Chen C J.Size dependent magnetic properties of iron oxide nanoparticles.J Magn Magn Mater, 2003,257:113 – 118.2, thermolysis and microemulsion method---the γ-Fe of preparation
2o
3often by tensio-active agent, be stabilized in organic solvent.Referring to Park J, An K J, Hwang Y S, et al.Ultra-large-scale syntheses of monodisperse nanocrystals.Nat Mater, 2004,3:891 – 895.3, solvent-thermal method---can well control the pattern of nano material, but synthesize γ-Fe with solvent-thermal method
2o
3often need High Temperature High Pressure.Referring to Sreeja V, Joy P A.Microwave-hydrothermal synthesis of γ-Fe
2o
3nanoparticles and their magnetic properties.Mater Res Bull, 2007,42:1570 – 1576.4, ultrasonic method---synthetic γ-Fe
2o
3need organic molysite, larger to environmental influence, but between its unique sound cavitation effect energy accelerated particle of ultrasonic method, collide with each other, reaction just can be carried out at normal temperatures.Referring to Ray I, Chakraborty S, Chowdhury A, et al.Room temperature synthesis of γ-Fe
2o
3by sonochemical route and its response towards butane.Sens Actuator B-Chem, 2007,130:882 – 888.But with the resulting γ-Fe of these methods
2o
3the size of nano particle is less, is all less than 50nm.Different application are to γ-Fe
2o
3pattern and size require different, for γ-Fe
2o
3application in fields such as biological medicine, sterilization, catalysis, the first, the size of general requirement sample and virus (20~500nm), protein (5~50nm), DNA (10~100nm) matches; The second, the γ-Fe of hollow structure
2o
3nanometer ball is because having larger specific surface area, lower density of material, good mechanics and thermal stability and higher surperficial permeability.Their hollow structure can provide the passage of delivery medicine, and becomes the optimal selection of the microcapsule carrier of medicine, for the γ-Fe of medicament transport
2o
3nano-hollow ball, if at room temperature there is superparamagnetism, can concentrate in destination organization and carry out medicament slow release by externally-applied magnetic field orientation, after removing externally-applied magnetic field, do not have remanent magnetism to interact, finally can get rid of (size is less than 5.5nm) by hepatic clearance and kidney.The 3rd, in the situation that changing magnetic field, γ-Fe
2o
3can there is pedesis and Neil relaxation mechanism in nano-hollow ball, produce heat and reach the thermotherapy temperature of cancer therapy.But preparation superparamagnetism γ-Fe
2o
3nano-hollow ball remains a huge challenge at present.
Summary of the invention
Goal of the invention
The object of the invention is to adopt laser liquid phase method to synthesize γ-Fe
2o
3nano-hollow ball.Utilize the advantage of laser preparation of nano material, a kind of environmental protection, pollution-free is provided, technique is simple, safe, synthetic γ-Fe that controllability is strong
2o
3the novel method of nano-hollow ball.
Technical scheme
A kind of laser liquid phase is prepared γ-Fe
2o
3the method of nano-hollow ball, is characterized in that: step is as follows:
(1) with nano level Fe
3o
4powder is raw material;
(2) raw material is carried out to strong acid treatment, after 5 to 10 minutes, carry out magnetic separation and be dispersed in iron nitrate solution, utilize ultrasonic wave to carry out supersound process to it, to form Fe
3o
4the mixed solution of powder, makes this mixed solution can be dispersed;
(3) use pulse laser bombardment Fe
3o
4mixed solution, laser beam converges at suspension surface, pulse laser wavelength is the pulse laser beam of 1.06 μ m, pulse width is 1.0ms, pulse-repetition is 10Hz, the laser power density of the zone of action is 10
5w/cm
2to 10
9w/cm
2, the lasing time is 1~3 hour;
(4) product pulse laser bombardment being obtained rinses centrifugal 3 times with acetone and water or other liquid medium respectively, finally at 60 ℃ of vacuum-drying 4h, obtains required sorrel sample.
The raw material Fe of described step (1)
3o
4for nano solid ball, median size is less than or equal to 150nm, and this solid nanometer ball is by secondary Fe
3o
4the unordered heap collective of crystal grain, secondary average grain size is less than or equal to 15nm.
The strong acid of described step (2) is nitric acid.
The laser bombardment of described step (3) adopts Nd:YAG solid statelaser.
In described step (3), to holding the reaction vessel of mixed solution, adopt the water-cooled mode of outer loop to absorb unnecessary heat, make liquid medium among normal temperature.
Other described liquid medium of step (4) is that deionized water or alcohol, ketone, ether can flowing fluids and the mixed solution of the arbitrary proportion that formed by arbitrary combination between them.
Advantage and effect
The present invention proposes a kind of laser liquid phase and prepare γ-Fe
2o
3the method of nano-hollow ball, tool has the following advantages:
Technique is simple, and lasing process safety is controlled, safety and environmental protection.γ-Fe
2o
3nano-hollow ball is at room temperature superparamagnetism, and has higher saturation magnetization and chemical stability.Magnetic γ-Fe
2o
3nano-hollow ball diameter range is 100~250nm, can be widely used in fields such as biomagnetism separation, living body detection, pharmaceutical carriers.
Accompanying drawing explanation
Fig. 1 is that laser liquid phase is prepared γ-Fe
2o
3the device schematic diagram of nano-hollow ball;
Fig. 2 is that laser liquid phase is prepared γ-Fe
2o
3the X ray electron-diffraction diagram of nano-hollow ball;
Fig. 3 is that laser liquid phase is prepared γ-Fe
2o
3the high power TEM photo of nano-hollow ball;
Fig. 4 is that laser liquid phase is prepared γ-Fe
2o
3the magnetzation curve of nano-hollow ball under 300K;
Fig. 5 is that laser liquid phase is prepared γ-Fe
2o
3nano-hollow ball is magnetzation curve under 5K.
Description of reference numerals:
1---laser apparatus, 2---pulse laser beam, 3---total reflection prism, 4---plus lens, 5---solution, 6---water coolant, 7---ultrasonic generator.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described further:
The present invention is that a kind of laser liquid phase is prepared γ-Fe
2o
3the method of nano-hollow ball, step is as follows:
(1) with nano level Fe
3o
4powder is raw material;
(2) raw material is carried out to strong acid treatment, after 5 to 10 minutes, carry out magnetic separation and be dispersed in iron nitrate solution, utilize ultrasonic wave to carry out supersound process to it, to form Fe
3o
4the mixed solution of powder, makes this mixed solution can be dispersed;
(3) use pulse laser bombardment Fe
3o
4mixed solution, laser beam converges at suspension surface, pulse laser wavelength is the pulse laser beam of 1.06 μ m, pulse width is 1.0ms, pulse-repetition is 10Hz, the laser power density of the zone of action is 10
5w/cm
2to 10
9w/cm
2, the lasing time is 1~3 hour;
(4) product pulse laser bombardment being obtained rinses centrifugal 3 times with acetone and water or other liquid medium respectively, finally at 60 ℃ of vacuum-drying 4h, obtains required sorrel sample.
The raw material Fe of described step (1)
3o
4for nano solid ball, median size is less than or equal to 150nm, and this solid nanometer ball is by secondary Fe
3o
4the unordered heap collective of crystal grain, secondary average grain size is less than or equal to 15nm.(source is referring to road apple, Zhang Jilin, Sun Dehui etc.Single Fe that disperses
3o
4synthetic and the sign of sub-micron ball.Chinese Journal of Inorganic Chemistry, 2010,26 (7): 1177~1182 or other business Fe
3o
4nano powder).
The strong acid of described step (2) is nitric acid.
The laser bombardment of described step (3) adopts Nd:YAG solid statelaser.
The device that the present invention adopts as shown in Figure 1, the pulse laser beam 2 being produced by Nd:YAG solid statelaser 1, after total reflection prism 3, through plus lens 4, converge, focus on the liquid level place of solution 5, and outside by 6 pairs of systems of recirculated cooling water, undertaken coolingly at it, utilize 7 pairs of systems of ultrasonic generator to carry out supersound process.
In described step (3), to holding the reaction vessel of mixed solution, adopt the water-cooled mode of outer loop to absorb unnecessary heat, make liquid medium among normal temperature.
Other described liquid medium of step (4) be deionized water or alcohol, ketone, ether etc. all can flowing fluid and the mixed solution of the arbitrary proportion that formed by arbitrary combination between them.
Specific embodiment is as follows:
1, by the Fe of the black of 20mg
3o
4solid sphere powder adds and is dissolved in the salpeter solution (HNO of 100mL2mol/L
3) in, Fe here
3o
4powder median size is 150nm, and magnetic is separated and be scattered in and contain 200mL0.5mol/L iron nitrate (Fe (NO after 5min
3)
3) in solution, utilize ultrasonic wave to carry out supersound process to it, to form Fe
3o
4the mixed solution of powder.
2, use the Fe of pulse laser implant steps 1
3o
4powder mixed solution, through HNO
3after processing, Fe
3o
4nanometer solid sphere surface has attached H
+, laser spot converges at through HNO
3dispersion liquid surface after processing, in laser light to the zone of action, Fe in laser bombardment process
3o
4the crystal grain generation oxicracking on nanometer solid sphere surface, has impelled the generation in part crystal grain gap; At Fe
3o
4in crystal grain, there is the Fe that outside rate of diffusion is larger
2+the H less with inside rate of diffusion
+, NO
3 –at both intersection generation redox reactions, the Fe of 150nm
3o
4in nanometer solid sphere, the Fe of secondary 15nm
3o
4grain oxidation cracking becomes γ-Fe of 5nm
2o
3, there is Kinkendal Effect in crystal grain, solid sphere starts to form γ-Fe by interior to inner
2o
3hollow structure, hollow ball γ-Fe
2o
3by γ-Fe
2o
3crystal grain is piled up and is formed.After laser bombardment 2h, Fe
3o
4be converted into γ-Fe completely
2o
3, formed nano-hollow sphere structuredly, median size is 200nm.
Laser power density in the focus zone of action of pulse laser is 10
5w/cm
2to 10
9w/cm
2, the lasing time is 2h.By Nd:YAG solid statelaser output wavelength, be the pulse laser beam of 1.06 μ m, pulse width 1.0ms, pulse-repetition is 10Hz.
Fe
3o
4powder mixed solution should guarantee in liquid medium dispersed.Due to the dissemination of ultrasonic wave to mixed solution, make laser not act in the same time different Fe
3o
4powder, is conducive to improve the productive rate of product.
In the process of bombardment, to holding the reaction vessel of mixed solution, adopt the water-cooled mode of outer loop to absorb unnecessary heat, make liquid medium among normal temperature.
3, by the ultrasonic 2h of product after bombardment, product is rinsed centrifugal 3 times with acetone and water respectively, finally at 60 ℃ of vacuum-drying 4h, obtain required sorrel.
In the same reaction unit, do not have the processing condition of explanation identical with embodiment 1.By Nd:YAG solid statelaser output wavelength, be the pulse laser beam (pulse width 1.0ms, pulse-repetition 20Hz) of 1.06 μ m, after total reflective mirror, optical lens converge, focus on the Fe through overpickling
3o
4the surface of powder mixed solution, liquid medium is iron nitrate (Fe (NO
3)
3) solution, mixed solution is utilized to ultrasonic dispersion.Adopt outer loop water-bath cooling the reaction vessel that holds mixed solution.Laser bombards 1h continuously, and product obtains sorrel powder through washing, after centrifugal, dry, and median size is 200nm.
Embodiment 3
In the same reaction unit, do not have the processing condition of explanation identical with embodiment 1.The pulse-repetition that changes pulse laser beam is pulse-repetition 10Hz.Liquid medium is iron nitrate (Fe (NO
3)
3) solution, mixed solution is utilized to ultrasonic dispersion, adopt outer loop water-bath cooling the reaction vessel that holds mixed solution.Laser bombards 1h continuously, and product obtains sorrel powder through washing, after centrifugal, dry, and median size is 200nm.
In the same reaction unit, do not have the processing condition of explanation identical with embodiment 1.The pulse-repetition that changes pulse laser beam is pulse-repetition 30Hz.Liquid medium is iron nitrate (Fe (NO
3)
3) solution, mixed solution is utilized to ultrasonic dispersion, adopt outer loop water-bath cooling the reaction vessel that holds mixed solution.Laser bombards 1h continuously, and product obtains sorrel powder through washing, after centrifugal, dry, and median size is 200nm.
Embodiment 5
In the same reaction unit, do not have the processing condition of explanation identical with embodiment 1.Only change laser and bombard continuously 3h, product obtains sorrel powder through washing, after centrifugal, dry, and median size is 210nm.
In the same reaction unit, do not have the processing condition of explanation identical with embodiment 1.Product obtains sorrel powder through washing, after centrifugal, dry.X-ray diffractometer (XRD) analysis shows, referring to Fig. 2.γ-the Fe of diffraction pattern and standard
2o
3(JCPDS No.39-1346, a=8.347~8.351
) peak position is consistent, according to γ-Fe
2o
3it is 8.3476 that nanocrystal diffraction pattern is tried to achieve cubic cell parameter
, according to Scherrer formula, from highest peak (311), calculate gained γ-Fe
2o
3the mean sizes of nanocrystal is 5nm.
Embodiment 7
In the same reaction unit, do not have the processing condition of explanation identical with embodiment 1.The pulse-repetition that only changes pulse laser is 10Hz, and laser bombards 3h continuously, and product obtains sorrel powder through washing, after centrifugal, dry, and median size is 200nm.Referring to Fig. 3.The TEM result of high power shows, in Fig. 2, the obvious electron density of black outer rim and white center is poor, has confirmed that prepared sample is nano-hollow ball, calculates the about 200nm of diameter of hollow structure, and shell thickness is approximately 50nm; XRD shows that hollow ball is the secondary γ-Fe that is 5nm by many size median sizes
2o
3nanocrystal forms, and γ-Fe is described
2o
3nano-hollow ball is polycrystalline phase; The TEM photo of high power has proved the existence of hollow ball microvoid structure, therefore resulting γ-Fe
2o
3nano-hollow ball has certain Drug loading capacity.
In the same reaction unit, do not have the processing condition of explanation identical with embodiment 1.Product obtains sorrel powder through washing, after centrifugal, dry, and median size is 200nm.Product is surveyed saturation magnetization with vibrating sample magnetometer, and the saturation magnetization 51emu/g under curve data show sample room temperature 300K, referring to Fig. 4.Than general γ-Fe
2o
3the large 20emu/g of nano particle.Can find out γ-Fe
2o
3at room temperature there is superparamagnetism, without hysteresis, without remanent magnetism or coercive force, exist.And in zero magnetic field, there is no hysteresis phenomenon, gained γ-Fe is described
2o
3nano-hollow ball at room temperature has superparamagnetism.During low temperature 5K, the saturation magnetization in 8kOe environment is 68emu/g, higher than room temperature.Referring to Fig. 5.Low temperature magnetic particle becomes the cold body of magnetic, and thermal motion reduces, and anisotropy performance strengthens, and makes the saturation magnetization of low temperature higher than room temperature.When temperature is 5K, curve is in a center of symmetry, has shown its superparamagnetic characteristic.
Embodiment 9
In the same reaction unit, do not have the processing condition of explanation identical with embodiment 1.Product obtains sorrel powder through washing, after centrifugal, dry, and median size is 200nm.By γ-Fe
2o
3nano-hollow ball is dispersed in rare nitric acid and deionized water, after externally-applied magnetic field, can be separated with the form of magnetic fluid, is removing magnetic field, through slight just rocking, can again be scattered in rare nitric acid and deionized water, and the γ-Fe of synthesized is described
2o
3nano-hollow ball can be scattered in acidity and the aqueous solution well, can not dissolved by diluted acid, and can in 48h, not produce sedimentation, shows that it has good chemical stability and dispersiveness.
Claims (6)
1. a laser liquid phase is prepared γ-Fe
2o
3the method of nano-hollow ball, is characterized in that: step is as follows:
(1) with nano level Fe
3o
4powder is raw material;
(2) raw material is carried out to strong acid treatment, after 5 to 10 minutes, carry out magnetic separation and be dispersed in iron nitrate solution, utilize ultrasonic wave to carry out supersound process to it, to form Fe
3o
4the mixed solution of powder, makes this mixed solution can be dispersed;
(3) use pulse laser bombardment Fe
3o
4mixed solution, laser beam converges at suspension surface, pulse laser wavelength is the pulse laser beam of 1.06 μ m, pulse width is 1.0ms, pulse-repetition is 10 Hz, the laser power density of the zone of action is 10
5w ∕ cm
2to 10
9w ∕ cm
2, the lasing time is 1~3 hour;
(4) product pulse laser bombardment being obtained rinses centrifugal 3 times with acetone and water or other liquid medium respectively, finally at 60 ℃ of vacuum-drying 4 h, obtains required sorrel sample.
2. laser liquid phase according to claim 1 is prepared γ-Fe
2o
3the method of nano-hollow ball, is characterized in that: the raw material Fe of described step (1)
3o
4for nano solid ball, median size is less than or equal to 150nm, and this solid nanometer ball is by secondary Fe
3o
4the unordered heap collective of crystal grain, secondary average grain size is less than or equal to 15 nm.
3. laser liquid phase according to claim 1 is prepared γ-Fe
2o
3the method of nano-hollow ball, is characterized in that: the strong acid of described step (2) is nitric acid.
4. laser liquid phase according to claim 1 is prepared γ-Fe
2o
3the method of nano-hollow ball, is characterized in that: the laser bombardment of described step (3) adopts Nd:YAG solid statelaser.
5. laser liquid phase according to claim 1 is prepared γ-Fe
2o
3the method of nano-hollow ball, is characterized in that: in described step (3), to holding the reaction vessel of mixed solution, adopt the water-cooled mode of outer loop to absorb unnecessary heat, make liquid medium among normal temperature.
6. laser liquid phase according to claim 1 is prepared γ-Fe
2o
3the method of nano-hollow ball, is characterized in that: other described liquid medium of step (4) is that deionized water or alcohol, ketone, ether can flowing fluids and the mixed solution of the arbitrary proportion that formed by arbitrary combination between them.
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Cited By (1)
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CN106830096A (en) * | 2017-02-28 | 2017-06-13 | 东南大学 | A kind of preparation method of magnetic Nano iron oxide |
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WO2011074587A1 (en) * | 2009-12-15 | 2011-06-23 | 国立大学法人岡山大学 | Magnetic ceramic and process for production thereof |
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2013
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CN1116976A (en) * | 1994-08-15 | 1996-02-21 | 中国科学院金属研究所 | Lasser gas-phase synthesis of gamma ferric oxide nanometer micropowder |
US7829140B1 (en) * | 2006-03-29 | 2010-11-09 | The Research Foundation Of The State University Of New York | Method of forming iron oxide core metal shell nanoparticles |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106830096A (en) * | 2017-02-28 | 2017-06-13 | 东南大学 | A kind of preparation method of magnetic Nano iron oxide |
CN106830096B (en) * | 2017-02-28 | 2018-04-24 | 东南大学 | A kind of preparation method of magnetic Nano iron oxide |
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