CN106867040A - A kind of β FeSi2Nanometer hexahedron particle Chitosan Composites and preparation method - Google Patents

A kind of β FeSi2Nanometer hexahedron particle Chitosan Composites and preparation method Download PDF

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CN106867040A
CN106867040A CN201710113825.8A CN201710113825A CN106867040A CN 106867040 A CN106867040 A CN 106867040A CN 201710113825 A CN201710113825 A CN 201710113825A CN 106867040 A CN106867040 A CN 106867040A
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nanometer
fesi
hexahedron
particle
film
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CN106867040B (en
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吴淑毅
单云
吴兴龙
沈剑沧
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Nanjing University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/40—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials of magnetic semiconductor materials, e.g. CdCr2S4
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00—Thin magnetic films, e.g. of one-domain structure
    • H01F10/007—Thin magnetic films, e.g. of one-domain structure ultrathin or granular films
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00—Thin magnetic films, e.g. of one-domain structure
    • H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
    • H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
    • H01F10/18—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being compounds
    • H01F10/193—Magnetic semiconductor compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/30—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates for applying nanostructures, e.g. by molecular beam epitaxy [MBE]
    • H01F41/301—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates for applying nanostructures, e.g. by molecular beam epitaxy [MBE] for applying ultrathin or granular layers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Abstract

The present invention relates to a kind of β FeSi2Nanometer hexahedron particle Chitosan Composites preparation method, anhydrous frerrous chloride and silicon chip are reacted under the conditions of 800 ± 10 DEG C, synthesis β FeSi2Nanometer hexahedron particle；The carboxyl chitosan aqueous solution of the configuration quality than 0.2 ± 0.03%；The water-soluble drop-coated of carboxyl chitosan is drawn in cubic granules film surface with liquid-transfering gun；Film after drop coating is placed in vacuum drying chamber, 20min is dried at room temperature, form compact laminated film, i.e. β FeSi2Nanometer hexahedron particle Chitosan Composites.Composite has enhanced room-temperature ferromagnetic, in the application aspects such as magnetic transducing, Semiconductor Spintronics, biologic medical all great potentials.

Description

A kind of β-FeSi2Nanometer hexahedron particle Chitosan Composites and preparation method
Technical field
The present invention relates to a kind of β-FeSi with enhanced room-temperature ferromagnetic2Nanometer hexahedron particle shitosan is combined The preparation method of material, belongs to magnetic semiconductor field.
Background technology
With continuing to develop for science and technology, semiconductor and magnetic material are widely applied.Semiconductor devices can be quick Ground processing information, and magnetic material by the holding of the direction of magnetization can under conditions of Non-energy-consumption storage information.If material Characteristic of semiconductor and magnetic can be integrated, it is possible to change existing semiconductor integrated circuit process information, magnetic material Expect the pattern of disk storage information.The computer core part made with magnetic semiconductor, while processing data, Ke Yijin The non-volatile memories of row data, even if power-off suddenly, data will not also lose.
With the development of semiconductor industry, the component number on VLSI chip is continuous according to Moore's Law Increase, channel length develops into nanometer scale from original micron dimension, leakage current increase, caloric value increase and parasitism can be brought The problems such as capacity effect, in addition, with the appearance of quantum Interference, the Performance And Reliability of device can be severely impacted. It is known that an electron is negatively charged, electric charge is the one degree of freedom of electronics；This exoelectron has magnetic, and spin is another of electronics The free degree.In general semiconductor electronics spin regulation and control get up it is extremely difficult, and in magnetic semiconductor magnetic atom spin only Plus an electric current or regulation and control need to be achieved that plus magnetic field.In addition the phase between the energy specific charge that interacts between spinning Interaction energy wants small 1000 times, changes spin and is more prone to.It is expected to develop data processing speed soon using magnetic semiconductor, consumption Electricity is low, and integrated level is high and New function semiconductor spin device of information Store " non-volatile ".
However, existing magnetic semiconductor Curie temperature is less than room temperature, although III-V race's dilute magnetic semiconductor realizes low temperature Antetype device function, but highest Curie temperature is also only 200K, it is impossible to meet practical application.Therefore, with intrinsic ferromagnetic The exploration discovery of magnetic semiconductor will carry out revolutionary impact to existing Structure of Information Industry banding.Our seminars are at this Persistent exploration is also carried out on problem in science, has synthesized the β-FeSi with room-temperature ferromagnetic2Nanocube (Z.Q.He et al.,J.Am.Chem.Soc.2015,137,11419–11424.).This material is in spintronics, information Store and biology Medical science (H.Lee et al., J.Am.Chem.Soc.2007,129,12739-12745；Y.Zhang et al., Adv.Mater.2016,28,1387-1393.) etc. aspect have potential application.If magnetism of material can be further enhanced, will Further expand material applications.We are β-FeSi2The magnetic of nano particle derives from surface, the local near surface iron atoms layer Magnetic moment can cause strong room-temperature ferromagnetic with the interaction of surface state itinerant electron.If can continue to increase fermi level The neighbouring spin density of states, is beneficial to the further increase of magnetic.There are some researches show by Fe3O4Nano material Graphene bag After wrapping up in, the ferromagnetism of composite construction enhance about 100emu/g (D.Seifuet al., Appl.Phys.Lett.2015, 106,212401-1–-5.)；The composite construction that organic molecule coated metal oxide is formed can be induced and strengthened at room temperature Ferromagnetism (M.A.Garcia et al., Nano Lett.2007,7,1489-1494；J.H.Zhang et al., Phys.Rev.B.2013,88,085437-1–-6.).Therefore, compound with organic molecule is to increase a kind of ferromagnetic effective means. If the biocompatibility that the organic molecule of selection has had, can further expand β-FeSi2Nano material is in biomolecule Detection, the application for carrying the aspects such as medicine, targeted therapy.Shitosan is natural macromolecular material, abundance, nontoxic and with spy Different physiologically active, stronger biocompatibility and good biodegradable, are the upper material selections of cladding.If can lead to Cross β-FeSi2Nano material and shitosan are combined to realize the enhancing of compound system magnetic, and this expansion to materials application will It is of great advantage.
The content of the invention
Present invention aim at, there is provided one kind enhancing β-FeSi2Simple, the effective side of nanometer hexahedron beads magnetic Method, prepares the composite with enhanced room-temperature ferromagnetic, good biocompatibility.
Technical scheme：β-FeSi2Nanometer hexahedron particle Chitosan Composites, anhydrous frerrous chloride is in silicon Piece surface is reacted under the conditions of 800 ± 10 DEG C, synthesis β-FeSi2Nanometer hexahedron particle, the carboxyl chitosan aqueous solution to β- FeSi2Nanometer hexahedron particle is combined, and forms composite material of core-shell structure.
The carboxyl chitosan aqueous solution of hexahedron nanometer particle film and 200 μ L is generated in the silicon chip plane of 1cm*1cm (mass concentration 0.2%) is combined, and forms composite material of core-shell structure.
Composite has the saturation magnetization of 157emu/g.
β-FeSi2Nanometer hexahedron particle Chitosan Composites and preparation method, anhydrous frerrous chloride and silicon chip are existed Reacted under the conditions of 800 ± 10 DEG C, synthesis β-FeSi2Nanometer hexahedron particle；Carboxylation shell of the configuration quality than 0.2 ± 0.03% gathers Sugar aqueous solution；The water-soluble drop-coated of carboxyl chitosan is drawn in cubic granules film surface with liquid-transfering gun；By the film after drop coating It is placed in vacuum drying chamber, 20min is dried at room temperature, forms compact laminated film, i.e. β-FeSi2Nanometer hexahedron Particle Chitosan Composites.
Hexahedron nanometer particle film is generated in the silicon chip plane of 1cm*1cm, liquid-transfering gun draws 0.2% carboxylic of 200 μ L Change chitosan aqueous solution drop coating in cubic granules film surface；Film after drop coating is placed in vacuum drying chamber, is dried 20min, forms compact composite film material.
Carboxyl chitosan (CS) used in the present invention, compared with polyaniline (PA) and perfluorinated sulfonic acid (Nafion), its official Can roll into a ball can occur stronger interaction with nano grain surface, more effectively increase the density of states that spinned near fermi level, Strengthen magnetic to a greater extent.As surface covers increasing for the amount of carboxyl chitosan, composite construction magnetic first gradually strengthens, and increases Gradually weaken again after to maximum.The carboxyl chitosan aqueous solution (the concentration of the hexahedron nanometer particle film of 1cm*1cm and 200 μ L 0.2%) it is combined, magnetic enhancement best results.
Beneficial effect of the present invention：It is related to a kind of β-FeSi with enhanced room-temperature ferromagnetic2Nanometer hexahedron particle shell Polysaccharide composite material and preparation method, the composite have the up to saturation magnetization of 157emu/g, enhancing before relatively wrapping up An order of magnitude.The material collection characteristic of semiconductor and magnetic have latent with all over the body in terms of spintronics and information Store In application.Additionally, the biocompatibility that the material has had, can also apply in terms of tumor imaging and biologic medical.
Brief description of the drawings
In Fig. 1, the hexahedron β-FeSi of drop coating different volumes carboxyl chitosan (CS) solution2The scanning of nanometer particle film Electron microscope picture, in figure:(a) 0 μ L carboxyl chitosan (CS) solution, (b) 100 μ L carboxyl chitosan (CS) solution, (c) 200 μ L carboxyl chitosans (CS) solution and (d) 300 μ L carboxyl chitosan (CS) solution.
(a) carboxyl chitosan (CS) and β-FeSi in Fig. 22The intensity of magnetization is with changes of magnetic field (M- before and after nano-particles reinforcement H) figure.B insertion figure is shitosan (CS) structural formula in the magnetic of () carboxyl chitosan (CS), (b).
Fig. 3 is heat treatment figure of the various concentrations carboxyl chitosan (CS) with nanometer particle film after compound.
(a) is polyaniline (PA) and β-FeSi in Fig. 42M-H figures before and after nano-particles reinforcement.The magnetic of (b) polyaniline (PA) Property, insertion figure is polyaniline (PA) structural formula.
(a) is perfluorinated sulfonic acid (Nafion) and β-FeSi in Fig. 52M-H figures before and after nano-particles reinforcement.(b) perfluorinated sulfonic acid (Nafion) magnetic, insertion figure is perfluorinated sulfonic acid (Nafion) structural formula.
Specific embodiment
A kind of β-FeSi with enhanced room-temperature ferromagnetic2Nanometer hexahedron particle Chitosan Composites and preparation side Method, the P-type silicon piece of the anhydrous frerrous chloride powder of 0.056g and 1cm*1cm is reacted at 800 DEG C ± 10 DEG C, synthesis β-FeSi2 The film of nanometer hexahedron particle composition；20mg carboxyl chitosans are weighed, in addition 10ml deionized waters, sonic oscillation 30 minutes Make to be uniformly dispersed；The water-soluble drop-coated of carboxyl chitosan of 200 μ L is drawn on hexahedron nanometer particle film surface with liquid-transfering gun；Will Film after drop coating is placed in vacuum drying chamber, and 20min is dried at 20 DEG C, forms compact laminated film.
Fig. 1 is the electron scanning micrograph of parcel different content carboxyl chitosan prepared by the present invention, it can be seen that As the increase of carboxyl chitosan content, film thickness increase, hexahedron particle gradually thickens, when chitosan content reaches During 300 μ L, surface has formed dense carboxyl chitosan film, and nano particle is fully wrapped around.
Fig. 2 is β-FeSi prepared by the present invention2The Magnetic Measurement figure of nanometer hexahedron particle Chitosan Composites.Will be multiple Close structure to be placed in superconducting quantum interference device (SQUID) (SQUID), added magnetic field is deducted parallel to silicon substrate, last hysteresis curve The diamagnetic signal of silicon substrate.It can be seen that, the saturation magnetization of nano particle is combined after 15emu/g, parcel before parcel The intensity of magnetization of structure increases to 157emu/g, enhances an order of magnitude or so.In order to exclude magnetic enhancement be initiated by it is used Carboxyl chitosan magnetic inherently, Magnetic Measurement has been also carried out to raw material carboxyl chitosan, is as a result shown as diamagnetic.These Result illustrates that we are derived from compound system at enhanced magnetic.Electric charge between the functional group of shitosan and surface iron atoms Transfer, has good regulating effect to the density of states that spinned at fermi level.
Increase ferromagnetic effect to probe into different content shitosan, we measure the compound of different content shitosan formation The magnetic of structure.Fig. 3 is the intensity of magnetization of part composite construction prepared by the present invention with the change curve in magnetic field.As parcel contains The increase of amount, the intensity of magnetization first increases and reduces afterwards, and when 200 μ L shitosans are wrapped up, enhancing effect is most notable.This shows with organic The increase of molecule content, the regulation and control of electric charge transfer between the two to the density of states that spinned at fermi level have fluctuation.
In order to probe into enhancing effect of the different functional groups to surface magnetism, we attempted other organic molecules and β- FeSi2Heat treatment situation after nanometer hexahedron Particles dispersed.Partial results are as shown in Figure 4 and Figure 5：The polyphenyl of optium concentration The compound rear system magnetic enhancement that amine is formed with nano particle is to 64emu/g, and perfluorinated sulfonic acid parcel is not almost appointed to magnetic What is contributed.Illustrate that different functional groups are acted on surface iron atoms, because bonding atomic electronegativity is different, charge transfer event is not Together, it is different to spin state density adjusting, cause final magnetic enhancement effect different.
To sum up explanation carboxyl chitosan can more effectively be acted on surface, and the enhancing effect to magnetic is optimal.

Claims (5)

1.β-FeSi2Nanometer hexahedron particle Chitosan Composites, it is characterized in that anhydrous frerrous chloride in silicon chip surface 800 Reacted under the conditions of ± 10 DEG C, synthesis β-FeSi2Nanometer hexahedron particle, the carboxyl chitosan aqueous solution is to β-FeSi2Nanometer hexahedron Particle is combined, and forms composite material of core-shell structure.
2. β-FeSi according to claim 12Nanometer hexahedron particle shitosan composite material of core-shell structure, it is characterized in that (quality is dense for the carboxyl chitosan aqueous solution of generation hexahedron nanometer particle film and 200 μ L in the silicon chip plane of 1cm*1cm 0.2%) degree is combined, and forms composite material of core-shell structure.
3. β-FeSi according to claim 12Nanometer hexahedron particle Chitosan Composites, it is characterized in that composite Saturation magnetization with 157emu/g.
4.β-FeSi2Nanometer hexahedron particle Chitosan Composites preparation method, it is characterized in that by anhydrous frerrous chloride and silicon chip Reacted under the conditions of 800 ± 10 DEG C, synthesis β-FeSi2Nanometer hexahedron particle；Carboxylation shell of the configuration quality than 0.2 ± 0.03% Water solution；The water-soluble drop-coated of carboxyl chitosan is drawn in cubic granules film surface with liquid-transfering gun；It is thin after by drop coating Film is placed in vacuum drying chamber, and 20min is dried at room temperature, forms compact laminated film, i.e. β-FeSi2Six faces of nanometer Body particle Chitosan Composites.
5. method according to claim 4, it is characterized in that generating hexahedron nano particle in the silicon chip plane of 1cm*1cm Film, liquid-transfering gun draws the water-soluble drop-coated of carboxyl chitosan of 0.2% 200 μ L in cubic granules film surface；By drop coating Film afterwards is placed in vacuum drying chamber, dries 20min, forms compact composite film material.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113813225A (en) * 2021-09-22 2021-12-21 中国科学院上海硅酸盐研究所 Portable beta-FeSi2Composite spray hydrogel and preparation method and application thereof

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US20100008854A1 (en) * 2008-07-11 2010-01-14 Seung Joo Haam Metal nanocomposite, preparation method and use thereof
CN103804720A (en) * 2012-11-06 2014-05-21 李征 Preparation method of magnetic carboxymethyled chitosan nanoparticles

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113813225A (en) * 2021-09-22 2021-12-21 中国科学院上海硅酸盐研究所 Portable beta-FeSi2Composite spray hydrogel and preparation method and application thereof
CN113813225B (en) * 2021-09-22 2023-01-10 中科硅肤康(济宁)医疗器械科技有限公司 Portable beta-FeSi 2 Composite spray hydrogel and preparation method and application thereof

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