CN104449682A - Preparation method of ZnS: Mn<2+>/Fe3O4 optomagnetic nanocomposite - Google Patents

Preparation method of ZnS: Mn<2+>/Fe3O4 optomagnetic nanocomposite Download PDF

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Publication number
CN104449682A
CN104449682A CN201410641567.7A CN201410641567A CN104449682A CN 104449682 A CN104449682 A CN 104449682A CN 201410641567 A CN201410641567 A CN 201410641567A CN 104449682 A CN104449682 A CN 104449682A
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aqueous solution
deionized water
preparation
composite material
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曹健
韩东来
杨景海
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Jilin Normal University
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Jilin Normal University
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Abstract

The invention belongs to the technical field of assembly of nanocomposites and relates to a preparation method of a ZnS: Mn<2+>/Fe3O4 optomagnetic nanocomposite. According to the preparation method, ZnS: Mn<2+> is subjected to surface modification by virtue of mercaptoacetic acid so that the surface of ZnS: Mn<2+> has carboxyl groups; Fe3O4 is subjected to surface modification by virtue of citric acid so that the surface of Fe3O4 has hydroxyl groups, by virtue of an electrostatic self-assembly method, ZnS: Mn<2+>(-COOH) and Fe3O4(-OH) are mixed at a certain proportion so that ZnS: Mn<2+> and Fe3O4 are bonded together by virtue of the action of covalent bonds to form the ZnS: Mn<2+>/Fe3O4 optomagnetic nanocomposite of which the size is only 10nm and which has excellent yellow luminescence and superparamagnetic property. The preparation method has the advantages of simple operation and environment friendliness and is economical and convenient and is easy to implement large-scale production.

Description

A kind of ZnS:Mn 2+/ Fe 3o 4the preparation method of optomagnetic nano composite material
Technical field
The invention belongs to the technical field of a kind of optomagnetic multifunctional nanocomposites preparation method, a kind of ZnS:Mn specifically 2+/ Fe 3o 4the packaging technology of optomagnetic nano composite material.
Background technology
21 century is century of nano science and life science, and the nanobiology that nano science and biology cross coupled are formed is one of the most vital developing direction.Utilization has optomagnetic multifunctional nano composite material as novel probe, presents application prospect widely in fields such as fluorescent mark, magnetic targeted, medicine controlled releasings.Wherein will there is the semiconductor nano material of excellent optical and there is the Fe of superparamagnetic character 3o 4nanomaterial assembly becomes optomagnetic nano composite material to become the study hotspot of people! In various semiconductor material, ZnS is a kind of very important II-VI group semiconductor material with wide forbidden band, has zink sulphide and wurtzite two kinds of structures, in ultraviolet light-emitting diode, flat-panel monitor, infrared window, sensor, the fields such as laser apparatus have important using value.Its energy band structure can be changed by carrying out ZnS adulterating, thus the photoelectric properties of ZnS semiconductor material and microtexture are very significantly improved, wherein ZnS:Mn 2+nano material has excellent yellow emission, and has higher fluorescence quantum efficiency and excellent light, thermostability, so ZnS:Mn 2+nano material has potential application prospect in fluorescent mark field.Fe 3o 4nano material has superparamagnetism, has good biocompatibility and stability, works as Fe 3o 4when the size of nano material is less than 10nm, sample has higher specific surface area and lower Curie temperature, therefore has huge using value in nuclear magnetic resonance, magnetic targeted release field.At present by ZnS:Mn 2+nano material and Fe 3o 4nano material is compounded to form the many employings of optomagnetic multifunctional nanocomposites increases transition layer between as SiO 2or the method for polymkeric substance avoids Fe 3o 4nano material is to ZnS:Mn 2+the fluorescence quenching of nano material, but prepared nano composite material size is often excessive, and packaging technology is complicated, length consuming time.Therefore the present invention discloses a kind of method of electrostatic self-assembled, achieves ZnS:Mn 2+/ Fe 3o 4the assembling of optomagnetic nano composite material, adopts surface modification technology, effectively improves ZnS:Mn 2+/ Fe 3o 4the stability of/nano composite material, reduces ZnS:Mn 2+/ Fe 3o 4the size of nano composite material, saves time and production cost greatly.
Summary of the invention
The object of this invention is to provide a kind of optomagnetic multi-functional ZnS:Mn 2+/ Fe 3o 4the preparation method of nano composite material.This packaging technology adopts a kind of method of electrostatic self-assembled, utilizes the covalently bound effect of finishing group to achieve undersized optomagnetic multi-functional ZnS:Mn 2+/ Fe 3o 4effective connection of nano composite material.
The object of the present invention is achieved like this, utilizes Thiovanic acid to ZnS:Mn 2+carry out finishing, make ZnS:Mn 2+surface, with carboxylic group-COOH, utilizes citric acid to Fe 3o 4carry out finishing, make Fe 3o 4surperficial with oh group-OH, by a certain proportion of ZnS:Mn 2+(-COOH) and Fe 3o 4(-OH) mixes, and carboxyl and hydroxyl generation dehydration reaction, make ZnS:Mn 2+and Fe 3o 4coupled together by the effect of covalent linkage, and size only has 10nm, sample has excellent light, magnetic property.
Concrete technical scheme of the present invention is as follows.
A kind of ZnS:Mn 2+/ Fe 3o 4the preparation method of optomagnetic nano composite material, has the ZnS:Mn of carboxyl modified 2+the preparation of the aqueous solution, the Fe of hydroxyl modified 3o 4the preparation of the aqueous solution and ZnS:Mn 2+/ Fe 3o 4the process of the assembling of nano composite material;
The ZnS:Mn of described carboxyl modified 2+the preparation of the aqueous solution, is specially: Zn (NO in mass ratio 3) 26H 2o: Mn (NO 3) 23H 2o=300: 0.18, the mol ratio thiocarbamide by material: metallic cation Zn 2+and Mn 2+summation=3: 1, weigh Zn (NO 3) 26H 2o, Mn (NO 3) 23H 2o, thiourea starting material; By Zn (NO 3) 26H 2o and Mn (NO 3) 23H 2o deionized water mixed room temperature stirs 1 hour, form mixed solution I, thiocarbamide and quadrol mixed room temperature are stirred 1 hour, form mixed solution I I, mixed solution I I to be joined in mixed solution I Keep agitation 2 hours, wherein deionized water, quadrol consumption are equal and by every gram of Zn (NO 3) 26H 2o respectively uses 80/3ml to calculate; Then put into reactor, 180 DEG C of reactions obtain the mixing solutions with white precipitate in 12 hours, and adopt deionized water and dehydrated alcohol to carry out ultrasonic cleaning, centrifugal twice to it respectively, drying obtains ZnS:Mn 2+white powder; By ZnS:Mn 2+join in deionized water, ultrasonic disperse 5 minutes stirring at room temperature 30 minutes, then instills Thiovanic acid (MPA) and continues stirring 1 hour, obtains ZnS:Mn 2+the aqueous solution of (-COOH), wherein the consumption of deionized water, Thiovanic acid (MPA) is by every milligram of ZnS:Mn 2+use 2ml respectively, 8 μ l calculate;
The Fe of described hydroxyl modified 3o 4the preparation of the aqueous solution, is specially: weigh FeCl 36H 2o, FeCl 24H 2o and Macrogol 4000 (PEG-4000), spent glycol mix and blend 30 minutes, then the ammoniacal liquor adding that concentration is 25%, be warmed up to 110 DEG C and stir 2 hours and condensing reflux, wherein, FeCl 36H 2o, FeCl 24H 2mass ratio=1.62 of O and Macrogol 4000: 1.99: 10, ethylene glycol and ammonia volume are by every gram of FeCl 24H 2o uses 125ml, 50ml to calculate respectively; Reaction stops the deionized water that utilizes after room temperature to be cooled to solution centrifugal, the ultrasonic pH=7.0 to solution, and 40 DEG C of vacuum-dryings obtain Fe in 48 hours afterwards 3o 4black powder; Take Fe 3o 4with etc. the citric acid of quality join in deionized water, ultrasonic disperse 10 minutes, stirs 1 hour, obtains Fe 3o 4the aqueous solution of (-OH), wherein deionized water consumption is by every milligram of Fe 3o 410.9ml is used to calculate;
Described ZnS:Mn 2+/ Fe 3o 4the assembling of nano composite material, is specially: by ZnS:Mn 2+the aqueous solution of (-COOH) joins Fe 3o 4stir 1 hour in the aqueous solution of (-OH), carry out centrifugal afterwards, 60 DEG C of vacuum-drying 3 hours, namely obtains target product, wherein ZnS:Mn 2+the aqueous solution of (-COOH) and Fe 3o 4the amount of aqueous solution used by volume=2: 25 of (-OH).
Advantage of the present invention:
1, the present invention adopts the method for electrostatic self-assembled, utilizes the covalently bound effect of finishing group to achieve undersized optomagnetic multi-functional ZnS:Mn 2+/ Fe 3o 4the preparation of nano composite material.Effectively reduce ZnS:Mn 2+/ Fe 3o 4the size of nano composite material, and there is yellow emission and superparamagnetic character, the nano composite material having fluorescent mark and magnetic targeted function and one for assembling concurrently provides important materials.
2, the present invention is not only simple to operate, and has environmental protection, economy, convenient, simple operation and other advantages, is easy to realize scale operation, simultaneously to prepare nano composite material size little for the method, optomagnetic performance good (see Fig. 4, Fig. 5), synthesis technique safety, has biocompatibility.
Accompanying drawing explanation
Fig. 1 is ZnS:Mn of the present invention 2+/ Fe 3o 4the process flow for assembling figure of nano composite material.
Fig. 2 is target product ZnS:Mn of the present invention 2+/ Fe 3o 4the X-ray diffractogram of nano composite material.
Fig. 3 is that prior art prepares CdS/Fe 3o 4the transmission electron microscope picture of nano composite material.
Fig. 4 is target product ZnS:Mn of the present invention 2+/ Fe 3o 4the transmission electron microscope picture of nano composite material.
Fig. 5 is target product ZnS:Mn of the present invention 2+/ Fe 3o 4the photoluminescence spectrogram of nano composite material.
Fig. 6 is target product ZnS:Mn of the present invention 2+/ Fe 3o 4the hysteresis graph of nano composite material.
Embodiment
Raw material required for the present invention, all purchased from Shenyang Chemical Reagent Co., Ltd., Sinopharm Group, is analytical reagent.
The ZnS:Mn of embodiment 1 carboxyl modified 2+the preparation of the aqueous solution
As shown in Figure 1: weigh Zn (NO in proportion 3) 26H 2o (0.3g), Mn (NO 3) 23H 2o (0.18mg), thiourea starting material, the mol ratio of various material is thiocarbamide: metallic cation (Zn 2+, Mn 2+) summation=3: 1.By Zn (NO 3) 26H 2o and Mn (NO 3) 23H 2o 8ml deionized water to be fully blended on magnetic stirring apparatus stirring at room temperature one hour, form mixed solution I, thiocarbamide 8ml quadrol to be fully blended on magnetic stirring apparatus stirring at room temperature one hour, form mixed solution I I, mixed solution I I to be joined in mixed solution I Keep agitation two hours, then the reactor of 20ml is put into, 180 DEG C of sintering, the mixing solutions with white precipitate is obtained after 12 hours, deionized water and dehydrated alcohol is adopted to carry out ultrasonic to it respectively, centrifugal twice, 80 DEG C of dryings 3 hours, take out sample afterwards, carry out XRD thing to test mutually, test result display ZnS:Mn 2+for hexagonal wurtzite structure, and without any dephasign.Weigh ZnS:Mn 2+(10mg), joined in 20ml deionized water, ultrasonic disperse 5 minutes, room temperature magnetic agitation 30 minutes, measures MPA (80 μ l) and is added dropwise in above-mentioned solution, continue stirring one hour, obtain ZnS:Mn 2+the aqueous solution of (-COOH), ZnS:Mn 2+the concentration of (-COOH) aqueous solution is 0.5mg/ml.
The Fe of embodiment 2 hydroxyl modified 3o 4the preparation of the aqueous solution
Weigh FeCl 36H 2o (1.62g), FeCl 24H 2o (1.99g) and PEG-4000 (10g) the abundant mixing machinery of 250ml ethylene glycol stir 30 minutes, measure concentration be 25% ammoniacal liquor (100ml) join in above-mentioned solution, be warmed up to 110 DEG C of mechanical stirring, this process needs two hours and condensing reflux, reaction stopping is to be cooled utilizes deionized water to solution centrifugal, ultrasonic several until the pH=7.0 of solution after room temperature, 40 DEG C of vacuum-dryings take out sample in 48 hours afterwards, carry out XRD thing to test mutually, test result is Fe 3o 4.Take Fe 3o 4(23mg) with citric acid (23mg), joined in 250ml deionized water, ultrasonic disperse ten minutes, mechanical stirring one hour, obtains Fe 3o 4the aqueous solution of (-OH).Fe 3o 4the concentration of (-OH) aqueous solution is 0.092mg/ml.
Embodiment 3ZnS:Mn 2+/ Fe 3o 4the assembling of nano composite material
By ZnS:Mn obtained for embodiment 1 2+the aqueous solution (20ml) of (-COOH) joins the obtained Fe of embodiment 2 3o 4in the aqueous solution (250ml) of (-OH), mechanical stirring one hour, is undertaken centrifugal by this solution, and namely 60 DEG C of vacuum-dryings obtain target product in 3 hours.Carry out XRD thing to test mutually, test result is shown as ZnS:Mn 2+/ Fe 3o 4nano composite material (see Fig. 2).
Embodiment 4ZnS:Mn 2+/ Fe 3o 4the pattern of nano composite material and performance
Adopt CdS/Fe prepared by prior art 3o 4the transmission electron microscope picture (see Fig. 3) of nano composite material, ZnS:Mn prepared by the present invention 2+/ Fe 3o 4the transmission electron microscope picture (see Fig. 4) of nano composite material, the as can be seen from Figure 3 CdS/Fe for preparing of prior art 3o 4nano composite material diameter is comparatively approximately 100nm.The ZnS:Mn for preparing of the present invention as can be seen from Figure 4 2+/ Fe 3o 4nano composite material diameter only 10nm, size reduces greatly.
Fig. 5 is ZnS:Mn prepared by the present invention 2+/ Fe 3o 4the Photoluminescence figure of nano composite material.Can be clear that target product of the present invention has yellow emission, and luminous intensity reaches 5000.This means, target product of the present invention has good photoluminescence performance, is suitable for biological fluorescent labelling application.
Fig. 6 is ZnS:Mn prepared by the present invention 2+/ Fe 3o 4the room temperature hysteresis graph of nano composite material.Can be clear that target product of the present invention has magnetic targeted, and saturation magnetization reaches 19emu/g.This means, target product of the present invention has stronger superparamagnetism, is suitable for biological target application.

Claims (1)

1. a ZnS:Mn 2+/ Fe 3o 4the preparation method of optomagnetic nano composite material, has the ZnS:Mn of carboxyl modified 2+the preparation of the aqueous solution, the F of hydroxyl modified e3o 4the preparation of the aqueous solution and ZnS:Mn 2+/ F e3o 4the process of the assembling of nano composite material;
The ZnS:Mn of described carboxyl modified 2+the preparation of the aqueous solution, is specially: Zn (NO in mass ratio 3) 26H 2o: Mn (NO 3) 23H 2o=300: 0.18, the mol ratio thiocarbamide by material: metallic cation Zn 2+and Mn 2+summation=3: 1, weigh Zn (NO 3) 26H 2o, Mn (NO 3) 23H 2o, thiourea starting material; By Zn (NO 3) 26H 2o and Mn (NO 3) 23H 2o deionized water mixed room temperature stirs 1 hour, form mixed solution I, thiocarbamide and quadrol mixed room temperature are stirred 1 hour, form mixed solution I I, mixed solution I I to be joined in mixed solution I Keep agitation 2 hours, wherein deionized water, quadrol consumption are equal and by every gram of Zn (NO 3) 26H 2o respectively uses 80/3ml to calculate; Then put into reactor, 180 DEG C of reactions obtain the mixing solutions with white precipitate in 12 hours, and adopt deionized water and dehydrated alcohol to carry out ultrasonic cleaning, centrifugal twice to it respectively, drying obtains ZnS:Mn 2+white powder; By ZnS:Mn 2+join in deionized water, ultrasonic disperse 5 minutes stirring at room temperature 30 minutes, then instills Thiovanic acid and continues stirring 1 hour, obtains ZnS:Mn 2+the aqueous solution of (-COOH), wherein the consumption of deionized water, Thiovanic acid is by every milligram of ZnS:Mn 2+use 2ml respectively, 8 μ l calculate;
The Fe of described hydroxyl modified 3o 4the preparation of the aqueous solution, is specially: weigh FeCl 36H 2o, FeCl 24H 2o and Macrogol 4000, spent glycol mix and blend 30 minutes, then the ammoniacal liquor adding that concentration is 25%, be warmed up to 110 DEG C and stir 2 hours and condensing reflux, wherein, FeCl 36H 2o, FeCl 24H 2mass ratio=1.62 of O and Macrogol 4000: 1.99: 10, ethylene glycol and ammonia volume are by every gram of FeCl 24H 2o uses 125ml, 50ml to calculate respectively; Reaction stops the deionized water that utilizes after room temperature to be cooled to solution centrifugal, the ultrasonic pH=7.0 to solution, and 40 DEG C of vacuum-dryings obtain Fe in 48 hours afterwards 3o 4black powder; Take Fe 3o 4with etc. the citric acid of quality join in deionized water, ultrasonic disperse 10 minutes, stirs 1 hour, obtains Fe 3o 4the aqueous solution of (-OH), wherein deionized water consumption is by every milligram of Fe 3o 410.9ml is used to calculate;
Described ZnS:Mn 2+/ Fe 3o 4the assembling of nano composite material, is specially: by ZnS:Mn 2+the aqueous solution of (-COOH) joins Fe 3o 4stir 1 hour in the aqueous solution of (-OH), carry out centrifugal afterwards, 60 DEG C of vacuum-drying 3 hours, namely obtains target product; Wherein ZnS:Mn 2+the aqueous solution of (-COOH) and Fe 3o 4the amount of aqueous solution used by volume=2: 25 of (-OH).
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CN109971480A (en) * 2017-12-27 2019-07-05 Tcl集团股份有限公司 A kind of composite nanometer particle and preparation method thereof

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CN106620716A (en) * 2016-11-20 2017-05-10 吉林师范大学 Composite hollow microsphere drug carrier with multiple functions of fluorescence visibility, magnetic targeting and pH sensitivity and preparation method of carrier
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Application publication date: 20150325