CN103203451A - Core-shell type La(1-x)SrxMnO3/Au nanometer composite particle and preparation method thereof - Google Patents
Core-shell type La(1-x)SrxMnO3/Au nanometer composite particle and preparation method thereof Download PDFInfo
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- CN103203451A CN103203451A CN2013100378985A CN201310037898A CN103203451A CN 103203451 A CN103203451 A CN 103203451A CN 2013100378985 A CN2013100378985 A CN 2013100378985A CN 201310037898 A CN201310037898 A CN 201310037898A CN 103203451 A CN103203451 A CN 103203451A
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Abstract
The invention belongs to the field of biological medicine materials and particularly relates to a core-shell type La(1-x)SrxMnO3/Au nanometer composite particle and a preparation method thereof. The nanometer composite particle uses Au as the shell and La(1-x)SrxMnO3 as the core, wherein 0.1<=x<=0.8, the diameter of the core is 5-50nm, the thickness of the Au core is 1-3nm, and a surface active agent is wrapped on the surface of the nanometer composite particle. By means of the method, the prepared nanometer particle simultaneously has excellent optical property and good magnetic property, and simultaneously, the problem that the existing LSMO nanometer particles have poor aqueous phase diffusivity and biocompatibility can be solved.
Description
Technical field
The invention belongs to biological medicine material field, particularly a kind of hud typed La
1-xSr
xMnO
3/ Au nano-complex particle and preparation method thereof.
Background technology
Studies show that magnetic nano-particle FeCo and SPIO nano particle (Fe3O4, γ-Fe2O3 or their derivative) etc. are used for magnetic thermotherapy (MHT) and are expected to become the effective means of the various cancers for the treatment of.But because their Curie temperature (Tc) is too high, in magnetic thermotherapy process, must heat up to avoid damaging normal tissue by implanting thermometer control.Recently, it is found that La
1-xSr
xMnO
3(LSMO, 0.175≤χ≤0.8) nano particle shows good ferromagnetism or soft iron magnetic, and its Curie temperature can be adjusted in the 371K scope at 283K by changing χ, at Curie temperature T
CBelow, the LSMO nano particle shows iron or contains the ferromagnetism behavior that they will become paramagnetism when being higher than this temperature, so far just can not heat again.Therefore, LSMO nano particle T
CA little more than 315K, can be used as the treatment temperature when too high fuse or in vivo as gauge tap.In addition, because the high electric conductivity of LSMO nano particle also can show the rate of heat addition of enhancing in the MHT process.The LSMO nano particle has been used as the very strong temperature control material of a kind of competitiveness and has begun to cause the concern of countries in the world.But at present the LSMO nano particle of preparation has greatly limited their range of application in the diffusivity of biocompatibility, aqueous phase, accurately control and have major defect aspect the temperature.
Summary of the invention
The object of the present invention is to provide a kind of novel hud typed La that has optics and magnetic property concurrently
1-xSr
xMnO
3/ Au nano-complex particle and preparation method thereof can be given LSMO nano particle good optical activity, solves the LSMO nano particle simultaneously in the diffusivity of aqueous phase and the problem of biologically active difference.
The technical solution used in the present invention is as follows:
Hud typed La
1-xSr
xMnO
3/ Au nano-complex particle, described nano-complex particle is with La
1-xSr
xMnO
3Be nuclear, 0.1≤χ≤0.8, nuclear diameter 5-50nm is shell with Au, Au thickness of the shell 1-3nm is coated with surfactant.
Described hud typed La
1-xSr
xMnO
3The preparation method of/Au nano-complex particle can followingly carry out: under the effect of PEO-PPO-PEO or PVP surfactant, prepare La earlier
1-xSr
xMnO
3Magnetic nano-particle is then at magnetic nano particle sub-surface parcel Au shell.
La preferably
1-xSr
xMnO
3The preparation method of magnetic nano-particle is as follows: be presoma with acetylacetone,2,4-pentanedione lanthanum or lanthanum acetate, manganese acetylacetonate or manganese acetate, acetylacetone,2,4-pentanedione strontium or strontium acetate, be surfactant with polyoxyethylene-poly-oxypropylene polyoxyethylene or polyvinylpyrrolidone, with 1,2-hexadecane glycol is reducing agent, be solvent with the octyl ether, adopt the nanometer micro-emulsion legal system to be equipped with nano-powder, obtain La behind the nano-powder 700-900 ℃ sintering
1-xSr
xMnO
3Nano particle.
Concrete, earlier with three kinds of presomas by a certain percentage with 1,2-hexadecane glycol and polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO) or polyvinylpyrrolidone evenly mix in octyl ether, in 1-2 h, mixture is heated to 100-120 ℃ and be incubated 1-2 h, is warmed up to 250-300 ℃ and the heating 48-72 h that refluxes in afterwards in 10 min; Product is carried out sintering after removing solvent, rises to 700-900 ℃ from room temperature within the 2h, then at 700-900 ℃ of calcining 10-12h, obtains the LSMO magnetic nano-particle.
Total amount in precursor is 1mmol, and the consumption of the solvent of adding is that the amount of substance of 10-30 ml, surfactant is 0.001-1mmol.
During parcel Au shell, with Au (ac)
3Or the chloric acid gold is presoma, is surfactant with polyoxyethylene-poly-oxypropylene polyoxyethylene or polyvinylpyrrolidone, carries out under the ultrasonic or stirring condition.
It is that presoma is prepared hud typed La by selecting the suitable polymer surfactant with the metal complex that the present invention adopts the nanometer micro-emulsion method first
1-xSr
xMnO
3/ Au nano-complex particle.
The present invention has given optical activity, biocompatibility and the chemical stability of magnetic nano-particle uniqueness by wrapping up nm of gold at the LSMO skin, thereby it is widely used in magnetic thermotherapy, temperature switch, medicine conveying and fields such as release, biology sensor and immunodiagnosis.
The nanometer micro-emulsion method the preparation field of nanoparticles in most critical be the selection of surfactant.Surfactant is a big class organic compound, is a kind of amphiphilic materials, and its structure is made up of two parts: lipophilic group and hydrophilic group, and the two ends, office form dissymmetrical structure.This unique parents' structure of surfactant has good adsorption, easily forms micella, can be used as stabilizing agent and comes the stabilized nanoscale material, but also have certain reduction, is widely used in nano material synthetic.The kind of surfactant is a lot, adopts among the present invention to have concurrently water-soluble and nontoxic, electroneutral polymer molecule polyoxyethylene-poly-oxypropylene polyoxyethylene PEO-PPO-PEO block copolymer biocompatibility are surfactant.PEO-PPO-PEO is the macromolecule that hydrophilic PEO segment and hydrophobic PPO segment is bound up with covalent bond, be molecule chain softness, good hydrophilic property, nontoxic, polyethers that biological safety is good, be the high molecular surfactant of a class nonionic, trade name is Pluronic.PEO is as hydrophilic segment among the Pluronic; it is a kind of polymer of nontoxic, hydrophilic, non-immunogenic; has excellent biocompatibility; be commonly used to the three-dimensional protective agent as various particulates; can avoid effectively and the immunoglobulin (Ig) effect; holdback carrier and phagocyte bind, and prolong the body-internal-circulation time of carrier.The shell of hydrophilic PEO block formation micella has been proved and can have stoped hematoblastic gathering, is fit to be applied to the pharmaceutical carrier field.Block copolymer not only can be self-assembled into the nano unit of form difference, size adjustable, and easily removes after the reaction, is a kind of good nano material template agent, is applied in the design building-up process of mesoporous material.Have good biocompatibility in addition, can carry out functional groups easily and modify, in biomaterial, be widely used.Block copolymer has the micelle voltinism matter that temperature relies on, it is grafted on biocompatibility macromolecule or the pH value sensitive high molecular weight, can present better character, such functional polymer can be applied to temperature sensing material and the directed pharmaceutical carrier aspect that discharges.Under certain Pressure, Concentration, Temperature, the Pluronic copolymer is spontaneous formation micella in the aqueous solution, and its hydrophobic segment PPO twines the formation hydrophobic cores mutually, and hydrophilic segment PEO then is looped around the outer pliable and tough hydrophily shell that forms.Hydrophobic inner core is the nanometer microreactor for the nucleation of nano particle and growth provide a stable little reaction environment, and because of its distinctive amphiphilic effect with stabilized nanoscale particle.The hydrophily shell makes that micella can be stable is present in the aqueous solution or body fluid.Therefore, the nano particle of Pluronic copolymer parcel is medically having good prospects for application.The PEO-PPO-PEO that the present invention adopts is specially PEO-PPO-PEO(Mav.5800).
PEO-PPO-PEO or the PVP of the present invention's preparation wrap up hud typed La
1-xSr
xMnO
3/ Au nano-complex particle has the following advantages:
1) has magnetics and optical property simultaneously concurrently;
2) Curie changes super sharp keen;
3) aqueous phase has good diffusivity;
4) narrow diameter distribution, degree of crystallinity height, composition and particle size are adjustable, and the Au shell thickness is adjustable;
5) bioaffinity good (the Au shell has bioaffinity);
6) based on Au shell character, easy and bioactive molecule coupling.
Preparation method of the present invention is simple, and solvent for use is environmentally friendly, is convenient to suitability for industrialized production.
The present invention has following advantage with respect to prior art:
The present invention is by the hud typed La of preparation
1-xSr
xMnO
3/ Au nano-complex particle makes nano particle have excellent optical property and good magnetic performance simultaneously concurrently, has solved the problem of existing LSMO nano particle water diffusivity and biocompatibility difference simultaneously.La
1-xSr
xMnO
3/ Au nano-complex particle has application potential at magnetic thermotherapy, phototherapy, medicine conveying and release, the pyromagnetic aspect such as switch that causes, and is biological, a kind of good material of field of medicaments.
Description of drawings
Fig. 1 makes the magnetometric analysis figure of composite nanoparticle for embodiment 1;
Fig. 2 makes the ultraviolet-visible absorption spectroscopy of composite nanoparticle in the aqueous solution for embodiment 1;
Fig. 3 makes the TEM of composite nanoparticle for embodiment 1;
Fig. 4 makes the HRTEM of composite nanoparticle for embodiment 1.
The specific embodiment
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1
1) with acetylacetone,2,4-pentanedione lanthanum (1.1989 mmol, 0.523 g), manganese acetylacetonate (1.7998 mmol, 0.6340g), three kinds of presomas of acetylacetone,2,4-pentanedione strontium (0.6010 mmol, 0.1718 g) add in the 250 ml there-necked flasks, add 1,2-hexadecane glycol (C again
14H
29CH (OH) CH
2(OH) (1.5 mmol, 0.3881 g), polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO) (0.0819 mmol, 0.4748g) and octyl ether (C
8H
17OC
8H
17, 95%) and (50 ml), magnetic agitation is evenly mixed;
2) in 2 h with 1) mixture that obtains is heated to 120 ℃ and be incubated 2 h, is warmed up to 300 ℃ and heating 72 h that reflux afterwards within 10 min rapidly.
3) the reaction gained nano-powder tube furnace of packing into after solvent is removed in centrifugation carries out sintering, rises to 800 ℃ from room temperature within the 2h, then at 800 ℃ of calcining 10h, obtains the LSMO magnetic nano-particle.
When 4) wrapping up the Au shell, in 100 ml alcohol solvents, mix 50 mg LSMO nano particles and 0.05 g polyoxyethylene-poly-oxypropylene polyoxyethylene surfactant under the room temperature, splash into 50 mg Au (ac) under stirring
3Alcohol saturated solution, constantly stir reaction down and carry out 8h and can make PEO-PPO-PEO and wrap up hud typed La
1-xSr
xMnO
3/ Au nano-complex particle.
The performance of the nano-complex particle that obtains is seen Fig. 1-4.
Nano particle changes the paramagnetism behavior into by the ferromagnetism behavior rapidly at about 320K as can be seen from Figure 1.Nano particle is spread in the water as can be seen from Figure 2 has tangible absworption peak about 262 nm and 600 nm, the absworption peak at 600 nm places can ascribe the surface plasma body resonant vibration of Au to, and the formation of Au shell has been described.The hud typed LSMO/Au nano-complex particle of Fig. 1,2 explanation the present invention preparations has excellent magnetics and optical property concurrently, has good diffusivity at water simultaneously.Can find out nano particle diameter narrowly distributing, the degree of crystallinity height that the present invention prepares from Fig. 3,4.
Embodiment 2
1) with acetylacetone,2,4-pentanedione lanthanum (1.1989 mmol, 0.523 g), manganese acetylacetonate (1.7998 mmol, 0.6340g), three kinds of presomas of acetylacetone,2,4-pentanedione strontium (0.6010 mmol, 0.1718 g) add in the 250 ml there-necked flasks, add 1,2-hexadecane glycol (C again
14H
29CH (OH) CH
2(OH) (1.5 mmol, 0.3881 g), polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO) (0.819 mmol, 4.748g) and octyl ether (C
8H
17OC
8H
17, 95%) and (100 ml), magnetic agitation is evenly mixed;
2) in 2 h with 1) mixture that obtains is heated to 120 ℃ and be incubated 2 h, is warmed up to 300 ℃ and heating 48 h that reflux rapidly within afterwards in 10 min.
3) the reaction gained nano-powder tube furnace of packing into after solvent is removed in centrifugation carries out sintering, rises to 900 ℃ from room temperature within the 2h, then 900 ℃ of calcinings 10, obtains the LSMO magnetic nano-particle.
When 4) wrapping up the Au shell, in 100 ml alcohol solvents, mix 50 mg LSMO nano particles and 0.05 g polyoxyethylene-poly-oxypropylene polyoxyethylene surfactant under the room temperature, splash into 25 mg Au (ac) under stirring
3Alcohol saturated solution, constantly stir reaction down and carry out 6 h and can make PEO-PPO-PEO and wrap up hud typed La
1-xSr
xMnO
3/ Au nano-complex particle.
Embodiment 3
1) with acetylacetone,2,4-pentanedione lanthanum (0.8999 mmol, 0.3926 g), manganese acetylacetonate (1.7998 mmol, 0.6340g), three kinds of presomas of acetylacetone,2,4-pentanedione strontium (0.8999 mmol, 0.2572 g) add in the 250 ml there-necked flasks, add 1,2-hexadecane glycol (C again
14H
29CH (OH) CH
2(OH) (1.5 mmol, 0.3881 g), polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO) (0.0819 mmol, 0.4748g) and octyl ether (C
8H
17OC
8H
17, 95%) and (50 ml), magnetic agitation is evenly mixed;
2) in 2 h with 1) mixture that obtains is heated to 120 ℃ and be incubated 2 h, is warmed up to 280 ℃ and heating 72 h that reflux rapidly within afterwards in 10 min.
3) the reaction gained nano-powder tube furnace of packing into after solvent is removed in centrifugation carries out sintering, rises to 700 ℃ from room temperature within the 2h, then at 700 ℃ of calcining 12h, obtains the LSMO magnetic nano-particle.
When 4) wrapping up the Au shell, in 100 ml alcohol solvents, mix 50 mg LSMO nano particles and 0.05 g polyoxyethylene-poly-oxypropylene polyoxyethylene surfactant under the room temperature, splash into 50 mg Au (ac) under stirring
3Alcohol saturated solution, constantly stir reaction down and carry out 8h and can make PEO-PPO-PEO and wrap up hud typed La
1-xSr
xMnO
3/ Au nano-complex particle.
Above-described embodiment is the preferred embodiment of the present invention, but embodiments of the present invention are not restricted to the described embodiments, and the change that other any the present invention of not deviating from does all should be the substitute mode of equivalence, is included within protection scope of the present invention.
Claims (6)
1. hud typed La
1-xSr
xMnO
3/ Au nano-complex particle is characterized in that, described nano-complex particle is with La
1-xSr
xMnO
3Be nuclear, 0.1≤χ≤0.8, nuclear diameter 5-50nm is shell with Au, Au thickness of the shell 1-3nm is coated with surfactant.
2. the described hud typed La of claim 1
1-xSr
xMnO
3The preparation method of/Au nano-complex particle is characterized in that, under the effect of PEO-PPO-PEO or PVP surfactant, prepares La earlier
1-xSr
xMnO
3Magnetic nano-particle is then at magnetic nano particle sub-surface parcel Au shell.
3. hud typed La as claimed in claim 2
1-xSr
xMnO
3The preparation method of/Au nano-complex particle is characterized in that, La
1-xSr
xMnO
3The preparation method of magnetic nano-particle is as follows: be presoma with acetylacetone,2,4-pentanedione lanthanum or lanthanum acetate, manganese acetylacetonate or manganese acetate, acetylacetone,2,4-pentanedione strontium or strontium acetate, be surfactant with polyoxyethylene-poly-oxypropylene polyoxyethylene or polyvinylpyrrolidone, with 1,2-hexadecane glycol is reducing agent, octyl ether is solvent, adopt the nanometer micro-emulsion legal system to be equipped with nano-powder, obtain La behind the nano-powder 700-900 ℃ sintering
1-xSr
xMnO
3Nano particle.
4. hud typed La as claimed in claim 3
1-xSr
xMnO
3The preparation method of/Au nano-complex particle, it is characterized in that, earlier with three kinds of presomas, 1,2-hexadecane glycol and polyoxyethylene-poly-oxypropylene polyoxyethylene or polyvinylpyrrolidone evenly mix in octyl ether, in 1-2 h, mixture is heated to 100-120 ℃ and be incubated 1-2 h, is warmed up to 250-300 ℃ and the heating 48-72 h that refluxes in afterwards in 10 min; Product is carried out sintering after removing solvent, rises to 700-900 ℃ from room temperature within the 2h, then at 700-900 ℃ of calcining 10-12h, obtains La
1-xSr
xMnO
3Magnetic nano-particle.
5. hud typed La as claimed in claim 4
1-xSr
xMnO
3The preparation method of/Au nano-complex particle is characterized in that, is 1mmol in total amount of precursor, and the consumption of the solvent of adding is that the amount of substance of 10-30 ml, surfactant is 0.001-1mmol.
6. as the arbitrary described hud typed La of claim 2-5
1-xSr
xMnO
3The preparation method of/Au nano-complex particle is characterized in that, during parcel Au shell, with Au (ac)
3Or the chloric acid gold is presoma, is surfactant with polyoxyethylene-poly-oxypropylene polyoxyethylene or polyvinylpyrrolidone, carries out under the ultrasonic or stirring condition.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1372335A (en) * | 2002-04-01 | 2002-10-02 | 武汉理工大学 | Process for preparing solid oxide giant magnet electric resistance material |
| CN101224907A (en) * | 2008-01-04 | 2008-07-23 | 西南交通大学 | Method for preparing nano lanthanum-strontium-manganese oxide |
| JP2008258601A (en) * | 2007-03-09 | 2008-10-23 | Toshiba Corp | Core-shell type magnetic particle, high-frequency magnetic material and magnetic sheet |
| CN101620910A (en) * | 2008-07-01 | 2010-01-06 | 中国科学院成都有机化学有限公司 | Preparation method and application of core-shell magnetic/gold nanocomposite particles |
| CN101789295A (en) * | 2009-12-22 | 2010-07-28 | 湖南大学 | Gold shell magnetic nanoparticles, preparation thereof and use thereof |
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2013
- 2013-01-31 CN CN201310037898.5A patent/CN103203451B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1372335A (en) * | 2002-04-01 | 2002-10-02 | 武汉理工大学 | Process for preparing solid oxide giant magnet electric resistance material |
| JP2008258601A (en) * | 2007-03-09 | 2008-10-23 | Toshiba Corp | Core-shell type magnetic particle, high-frequency magnetic material and magnetic sheet |
| CN101224907A (en) * | 2008-01-04 | 2008-07-23 | 西南交通大学 | Method for preparing nano lanthanum-strontium-manganese oxide |
| CN101620910A (en) * | 2008-07-01 | 2010-01-06 | 中国科学院成都有机化学有限公司 | Preparation method and application of core-shell magnetic/gold nanocomposite particles |
| CN101789295A (en) * | 2009-12-22 | 2010-07-28 | 湖南大学 | Gold shell magnetic nanoparticles, preparation thereof and use thereof |
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