CN101168804A - One-dimensional CdS-Ni semiconductor-magnetic functional composite nano material and preparation method thereof - Google Patents
One-dimensional CdS-Ni semiconductor-magnetic functional composite nano material and preparation method thereof Download PDFInfo
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- CN101168804A CN101168804A CNA2007101148383A CN200710114838A CN101168804A CN 101168804 A CN101168804 A CN 101168804A CN A2007101148383 A CNA2007101148383 A CN A2007101148383A CN 200710114838 A CN200710114838 A CN 200710114838A CN 101168804 A CN101168804 A CN 101168804A
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Abstract
The invention relates to a single dimensional CdS-Ni semiconductor-magnetic function compound nano material and the preparation method thereof, and belongs to the inorganic nano material preparation field. The preparation method of the single dimensional CdS-Ni semiconductor-magnetic function compound nano material mainly comprises the preparation of the CdS nano line, and the heterochronous assembly of the CdS nano lines and the Ni nano grains based on the preparation of the CdS nano line. The design of the invention is rational, the operation is simple, the reaction is easy to control and the repeatability is good; the phase of the obtained phase is pure, the average diameter of the semiconductor CdS nano line is 35 nanometers, the length is about a plurality of nanometers, and the average diameter of each magnetic Ni grain is 50 nanometers. Through the magnetic modification to the single dimensional semiconductor CdS nano structure, the direction and the position can be conveniently controlled through the magnetic field, thereby solving the difficult problem that the nano material is difficult to recover, etc.
Description
Technical field:
The present invention relates to one-dimensional CdS-Ni semiconductor-magnetic functional composite nano material and preparation method thereof, belong to field of inorganic nano-material preparation.
Background technology:
The one-dimensional inorganic semiconductor nano material is because anisotropy, quantum size effect, surface effects and the dielectric confinement effect of shape, have the new features that are different from nano particle, have extremely important status at various transmitters, microtool, microelectrode, device integrated connecting line and follow-on display device etc.Calendar year 2001, thought an important breakthrough by " science " magazine (SCIENCE.2003,291,1941.) with the nanometer circuit that semiconductor nanowires is made.2006, Wang Zhonglin reported a kind of nano generator (SCIENCE, 2006,312,242.).Atomic force microscope probe is contacted with the ZnO array, make the nano wire bending,, have the probe of metallic membrane and nano wire to form the Schottky potential barrier, thereby produce electric current because the coupling of the piezoelectricity of ZnO nano wire and semiconductor property produces stress field and charge distribution.This discovery will make many nano-devices self that power can be provided, and not need battery, and the integrated nanosystems sizes of related device such as making light, electricity, biosensor is dwindled greatly.
As a kind of typical photoelectric semiconductor material, Nano cadmium sulphide has narrower energy gap (Eg=2.5ev), to the visible light sensitivity, tempting application prospect is arranged at aspects such as photoabsorption, photoluminescence, opto-electronic conversion, nonlinear optics, photochemical catalysis, biomarker and transmitters.The characteristic of research one dimension semiconductor CdS nano material aspect light, electric work energy, and utilize the whole bag of tricks that the CdS nano-material surface is carried out modification, function assembling etc., make it in application, to have better performance, become the focus of present functionalization cadmium sulfide nano material synthesis technology research.One dimension semiconductor CdS nanostructure is widely used in preparing very sensitive device, but entire device making processes is loaded down with trivial details, success ratio is low, and need relate to expensive main equipment, such as utilizing photoetching technique to prepare electrode, utilizing focused particle beam to carry out microwelding or the like.Prior problem is in the nano-device preparation process, to be difficult to realize to the direction of single one-dimensional CdS nanostructure and the accurate control of position thereof.Therefore we expect, modify by one dimension semiconductor CdS nanostructure being carried out magnetic, thereby can utilize magnetic field that its direction and position are handled easily, can solve nano material and be difficult to difficult problems such as recovery, aspect practical application, have the meaning of particularly important.
Summary of the invention:
At the deficiencies in the prior art, the invention provides the method that a kind of substep prepares one-dimensional CdS-Ni semiconductor-magnetic functional composite nano material.
The preparation method of one-dimensional CdS-Ni semiconductor-magnetic composite nano materials comprises the preparation of homogeneous CdS nano wire and the heterogeneous assembling of CdS nano wire and Ni nano particle, and step is as follows:
(1) preparation scale homogeneous CdS nano wire
Take by weighing 0.4g CdCl
22.5H
2O and 0.8g Tong Shiji are dissolved in respectively in the 20mL water, and the two mixes, and stir under the room temperature 10-30 minute, filter to collect to obtain white product, after the white product room temperature water is given a baby a bath on the third day after its birth time, place 70 ℃ of dry 10-15 of electric heating constant temperature heating container hours.Getting above-mentioned gained sample 1g places in the stainless steel cauldron of the inner liner polytetrafluoroethylene that the 45mL quadrol is housed, reactor is tightened in sealing, under 100 ℃～300 ℃ constant temperatures, react 24～72h, after reaction finishes, naturally cool to room temperature, with washing respectively under the products therefrom room temperature, alcohol washes twice, centrifugation and at 70 ℃ of dry 10-15 hours then promptly obtains yardstick homogeneous CdS nano wire.
(2) the heterogeneous assembling of CdS nano wire and Ni nano particle prepares the one-dimensional CdS-Ni semiconductor-magnetic composite nano materials
Get homogeneous CdS the nano wire, (NiCl of 0.062g～0.124g) of 0.03g step (1) preparation
26H
2The O, (N of 0.24g～0.64g)
2H
4H
2The NaOH solution of O and 1mol/L places in the stainless steel cauldron of the inner liner polytetrafluoroethylene that 45mL ethylene glycol/distilled water mixed solvent is housed, stirred 10-30 minute under the room temperature, reactor is tightened in sealing, isothermal reaction 5～30h under 60 ℃～180 ℃ conditions, after reaction finishes, naturally cool to room temperature, with washing, alcohol are washed twice respectively under the products therefrom room temperature, centrifugation and at 70 ℃ of dry 10-15 hours then, promptly obtain the one-dimensional CdS-Ni semiconductor-magnetic composite nano materials, the volume ratio of described ethylene glycol and distilled water is 5: 1.Isothermal reaction described in step (1) and (2) is that reactor is placed in the baking oven of energy accurate temperature controlling.
The present invention is reasonable in design, and is simple to operate, easy control of reaction, good reproducibility; The products therefrom thing is mutually pure, and the mean diameter of CdS semiconductor nano wire is about 35 nanometers, the several approximately microns of length, and magnetic Ni average diameter of particles is 50 nanometers.
The thing of product is mutually by X-ray diffraction spectra (XRD) test, and adopting Bruker D8X-x ray diffractometer x is that diffraction light sources is made X light diffracting analysis to product with Cu-K alpha-ray (wavelength X=1.54178 ).
Fig. 1 a is the cadmium sulfide nano wires X-ray diffraction spectra of reaction 50h preparation under 200 ℃ of constant temperatures.Wherein spike can index be the diffraction peak of six sides (hcp) Cadmium Sulfide, its lattice parameter a=4.1319 , be in close proximity to the numerical value a=4.132 that standard card (JCPDS card no.65-3414) is reported, stronger diffraction peak shows that the crystallinity of prepared CdS nano wire is better.Fig. 1 b is NiCl
26H
2O gets 0.093g, N
2H
4H
2The part that reaction 30h obtains when O gets 0.48g and under 160 ℃ of constant temperatures coats the XRD diffraction pattern of the one-dimensional CdS-Ni composite nano materials of Ni nano particle, wherein the diffraction peak located of (111), (200), (220) can index be the Ni of face-centered cubic (fcc), and wherein (200) its 2 θ=51.847 of diffraction peak of locating ° overlap with six side's Cadmium Sulfides, 2 θ=51.881 ° of peaks of locating.
The pattern of product shows by transmission electron microscope photo (TEM), adopts Hitachi model H-700 transmission electron microscope, and acceleration voltage is 100kV.
Fig. 2 a is the panorama TEM photo of CdS nano wire, and as can be seen from the figure product is made up of the homogeneous nano wire of diameter 30～40 nanometers, a length hundreds of micron.Coated one deck nano nickel particles by halves on the surface of CdS nano wire as can be seen from Fig. 2 b, particle diameter is about 50 nanometers, by observing the existence that does not have to find free nickel nano particle.
From product TEM photo Fig. 3 after the effect of external magnetic field as seen, we can utilize magnetic field that its direction and arrangement position are handled easily.
The present invention carries out Heterogeneous Composite by CdS semiconductor and the magnetic Ni nano structural material with the difference in functionality characteristic, can utilize magnetic field easily the CdS semiconductor nano wire to be handled, can solve that nano material is difficult to difficult problems such as recovery in the practical application, lay a good foundation for developing novel high-effect microelectronic device, important use is arranged in fields such as biomedicine, electronics, environmental protection.
Description of drawings:
Fig. 1 is the X-ray diffraction spectra (XRD) of CdS nano wire and one-dimensional CdS-Ni semiconductor-magnetic functional composite nano material.
Fig. 2 is the transmission electron microscope photo (TEM) of typical CdS nano wire and one-dimensional CdS-Ni semiconductor-magnetic composite nano materials.
Fig. 3 is the transmission electron microscope photo of one-dimensional CdS-Ni semiconductor-magnetic composite nano materials after the effect of external magnetic field.
Embodiment:
The present invention will be further described below in conjunction with embodiment, but be not limited thereto.
Embodiment 1: the preparation method of above-mentioned one-dimensional CdS-Ni semiconductor-magnetic composite nano materials, mainly comprise the preparation of homogeneous CdS nano wire and the heterogeneous assembling of CdS nano wire and Ni nano particle on this basis, and the processing step of concrete preparation is as follows:
(1) takes by weighing 0.4g CdCl
22.5H
2O and 0.8g Tong Shiji are dissolved in respectively in the 20mL water, and the two mixes, and stir under the room temperature 10 minutes, filter to collect to obtain white product, after the white product room temperature water is given a baby a bath on the third day after its birth time, place 70 ℃ of dryings of electric heating constant temperature heating container 10 hours.Getting above-mentioned gained sample 1g places in the stainless steel cauldron of the inner liner polytetrafluoroethylene that the 45mL quadrol is housed, reactor is tightened in sealing, under 200 ℃ of constant temperatures, react 50h, after reaction finishes, naturally cool to room temperature, with washing respectively under the products therefrom room temperature, alcohol washes twice, centrifugation and 70 ℃ of dryings 10 hours then promptly obtains yardstick homogeneous CdS nano wire.
(2) preparation one-dimensional CdS-Ni semiconductor-magnetic composite nano materials
Get homogeneous CdS nano wire, the 0.093g NiCl of 0.03g step (1) preparation
26H
2O, 0.48g N
2H
4H
2The NaOH solution of O and 1mol/L is dispersed in the stainless steel cauldron of the inner liner polytetrafluoroethylene that 45mL ethylene glycol/distilled water mixed solvent is housed, stirred 10 minutes under the room temperature, reactor is tightened in sealing, isothermal reaction 30h under 160 ℃ of conditions, after reaction finishes, naturally cool to room temperature, with washing, alcohol are washed twice respectively under the products therefrom room temperature, centrifugation and 70 ℃ of dryings 10 hours then, promptly obtain the one-dimensional CdS-Ni semiconductor-magnetic composite nano materials, the volume ratio of described ethylene glycol and distilled water is 5: 1.
Embodiment 2:
Preparation process is with example 1, and difference is: preparation CdS nano wire isothermal reaction 30h under 150 ℃ of conditions
Embodiment 3:
Preparation process is with example 1, and difference is: preparation CdS nano wire isothermal reaction 30h under 250 ℃ of conditions.
Embodiment 4:
Preparation process is with example 1, and difference is: get 0.062g NiCl
26H
2O, 0.24g N
2H
4H
2O is dispersed in ethylene glycol/distilled water mixed solvent.
Embodiment 5:
Preparation process is with example 1, and difference is: get 0.124g NiCl
26H
2O, 0.64g N
2H
4H
2O is dispersed in ethylene glycol/distilled water mixed solvent.
Embodiment 6:
Preparation process is with example 1, and difference is: preparation one-dimensional CdS-Ni semiconductor-magnetic composite nano materials isothermal reaction 30h under 60 ℃ of conditions.
Embodiment 7:
Preparation process is with example 1, and difference is: preparation one-dimensional CdS-Ni semiconductor-magnetic composite nano materials isothermal reaction 30h under 100 ℃ of conditions.
Embodiment 8:
Preparation process is with example 1, and difference is: preparation one-dimensional CdS-Ni semiconductor-magnetic composite nano materials isothermal reaction 30h under 140 ℃ of conditions.
Claims (2)
1. the preparation method of an one-dimensional CdS-Ni semiconductor-magnetic composite nano materials mainly comprises the preparation of homogeneous CdS nano wire and the heterogeneous assembling of CdS nano wire and Ni nano particle, and the processing step of concrete preparation is as follows:
(1) preparation scale homogeneous CdS nano wire
Take by weighing 0.4g CdCl
22.5H
2O and 0.8g Tong Shiji are dissolved in respectively in the 20 mL water, and the two mixes, and stir under the room temperature 10-30 minute, filter to collect to obtain white product, after the white product room temperature water is given a baby a bath on the third day after its birth time, place 70 ℃ of dry 10-15 of electric heating constant temperature heating container hours.Getting above-mentioned gained sample 1g places in the stainless steel cauldron of the inner liner polytetrafluoroethylene that the 45mL quadrol is housed, reactor is tightened in sealing, under 100 ℃～300 ℃ constant temperatures, react 24～72h, after reaction finishes, naturally cool to room temperature, with washing respectively under the products therefrom room temperature, alcohol washes twice, centrifugation and at 70 ℃ of dry 10-15 hours then promptly obtains yardstick homogeneous CdS nano wire;
(2) the heterogeneous assembling of CdS nano wire and Ni nano particle prepares the one-dimensional CdS-Ni semiconductor-magnetic composite nano materials
Get homogeneous CdS the nano wire, (NiCl of 0.062g～0.124g) of 0.03 g step (1) preparation
26H
2The O, (N of 0.24g～0.64g)
2H
4H
2The NaOH solution of O and 1mol/L places in the stainless steel cauldron of the inner liner polytetrafluoroethylene that 45mL ethylene glycol/distilled water mixed solvent is housed, stirred 10-30 minute under the room temperature, reactor is tightened in sealing, isothermal reaction 5～30h under 60 ℃～180 ℃ conditions, after reaction finishes, naturally cool to room temperature, with washing, alcohol are washed twice respectively under the products therefrom room temperature, centrifugation and at 70 ℃ of dry 10-15 hours then, promptly obtain the one-dimensional CdS-Ni semiconductor-magnetic composite nano materials, the volume ratio of described ethylene glycol and distilled water is 5: 1.
2. the preparation method of a kind of one-dimensional CdS-Ni semiconductor-magnetic composite nano materials as claimed in claim 1 is characterized in that, the isothermal reaction described in described step (1) and (2) is that reactor is placed in the baking oven of energy accurate temperature controlling.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103128305A (en) * | 2011-11-28 | 2013-06-05 | 同济大学 | Method for preparing Ag/Co magnetic nano composites |
| CN104988475A (en) * | 2015-06-03 | 2015-10-21 | 南京理工大学 | Copper-nickel alloy nanowire flexible electrode and preparation method thereof |
| CN115318307A (en) * | 2022-08-29 | 2022-11-11 | 四川启睿克科技有限公司 | Method for designing high-performance hydrogen production cocatalyst by introducing galvanic couple layer and constructing snowflake-shaped CuNi @ EDL/CdS catalyst |
-
2007
- 2007-11-29 CN CNB2007101148383A patent/CN100480407C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103128305A (en) * | 2011-11-28 | 2013-06-05 | 同济大学 | Method for preparing Ag/Co magnetic nano composites |
| CN103128305B (en) * | 2011-11-28 | 2015-03-04 | 同济大学 | Method for preparing Ag/Co magnetic nano composites |
| CN104988475A (en) * | 2015-06-03 | 2015-10-21 | 南京理工大学 | Copper-nickel alloy nanowire flexible electrode and preparation method thereof |
| CN115318307A (en) * | 2022-08-29 | 2022-11-11 | 四川启睿克科技有限公司 | Method for designing high-performance hydrogen production cocatalyst by introducing galvanic couple layer and constructing snowflake-shaped CuNi @ EDL/CdS catalyst |
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Granted publication date: 20090422 Termination date: 20111129 |