CN1280457C - Wet-solid phase reaction preparation method for cadmium sulfide semiconductor nanocrystalline - Google Patents
Wet-solid phase reaction preparation method for cadmium sulfide semiconductor nanocrystalline Download PDFInfo
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- CN1280457C CN1280457C CN 200410041158 CN200410041158A CN1280457C CN 1280457 C CN1280457 C CN 1280457C CN 200410041158 CN200410041158 CN 200410041158 CN 200410041158 A CN200410041158 A CN 200410041158A CN 1280457 C CN1280457 C CN 1280457C
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Abstract
The present invention relates to a wet-solid phase reaction preparation method for cadmium sulfide semiconductor nanocrystals, which comprises the following steps: mercaptoacetic acids and cadmium chloride are mixed according to the molar ratio of 1.8 to 2.2:1, and ground. Deionizing water is added, the excessive mercaptoacetic acids are washed away and filtrated; filter cake is washed by the deionizing water; the filter cake and sodium sulfide are mixed according to the molar ratio of 1 to 3.5:2 and ground, and light yellow solids are obtained; the light yellow solids obtained at the former step are dissolved in water, and added in acetone or ether so that CdS collosol is deposited; the light yellow solids are filtrated, washed and dried; finally, CdS nanocrystals are obtained. The present invention has the advantages of proper reaction condition, simple technology, high yield, uniform particle diameter of the prepared particles, no agglomeration and favorable reproducibility. Compared with the traditional bioluminescence probe (organic dyes), the nanocrystals have the advantages of wide excitation spectrum, continuous distribution, symmetrical distribution of emission spectrums, narrow width of the emission spectrums, and adjustable colors; when the nanocrystals are used for bioluminescence probes, the nanocrystals have favorable development and application prospects.
Description
Technical field
The present invention relates to a kind of Cadmium Sulfide (CdS) preparation of nano crystal, particularly a kind of wet solid state reaction preparation method of the CdS nanocrystal as biological fluorescent labeling.
Background technology
CdS is the II-VI family photoelectric semiconductor material of a quasi-representative, it has purposes widely at aspects such as photodiode, solar cell, photochemical catalysis, nonlinear optical material, transmitter and information storage, and the CdS semiconductor nano material is the focus that people study all the time.The CdS semiconductor nano material is used for the bioprobe aspect and is gradually that also people pay close attention in recent years.Preparation CdS semiconductor nano material research at present is mainly by methods such as solvent thermal reaction, electrochemical deposition, sol-gels.Although these methods all have its advantage, it is present still very limited to prepare the CdS nano material with better water soluble characteristic and biomacromolecule effect, and it is necessary to explore new other the easy relatively method for preparing the CdS nano material of development.
Fluorescence spectrum is used comparatively extensive, wherein even more important with the mensuration of Yeast Nucleic Acid (RNA) and thymus nucleic acid (DNA) in biomedical and life science.But if directly when with fluorescent spectrometry they being studied, the fluorescence quantum yield of base and nucleic acid is very low, therefore detects their best method and still utilizes various fluorescent probes.At present, using the most general fluorescent probe is organic dye, in most of the cases, because their excitation spectrum is all narrower, so be difficult to the simultaneous excitation various ingredients, and its fluorescent characteristics is composed broad, and it is asymmetric to distribute, this brings difficulty for again the fluorescence of distinguishing the different probe molecule, therefore will detect comparatively difficulty of various ingredients simultaneously.The most serious defective of organic dye still is that photochemical stability is poor, and the fluorescent photon average quantity that photobleaching and photodissociation can be sent each probe dye can not be too many, and photolytic product tends to again organism is produced lethal effect.Utilize nanoparticle just can address these problems preferably as biological fluorescent labeling.Compare with traditional fluorescent probe, the exciting light spectrum width of nanocrystal, and continuous distribution, and emmission spectrum is symmetrical distribution and width is narrow, color tunable, the optical excitation of nanocrystalline physical efficiency coverlet one wavelength of promptly different sizes and send the light and the photochemical stability height of different colours is difficult for plurality of advantages such as photodissociation.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have that energy consumption is little, reaction conditions is gentle, technology is simple, the productive rate height, and the particle diameter of preparation is even, no agglomeration, the Nano cadmium sulphide preparation method of characteristics such as favorable reproducibility.Because finishing has Thiovanic acid, thereby solved the preparation method of Nano cadmium sulphide of the water-soluble and Bc of Nano cadmium sulphide crystalline substance well.
Technical solution of the present invention is that the wet solid state reaction preparation method that CdS semiconduct is nanocrystalline may further comprise the steps:
With Thiovanic acid and Cadmium chloride fine powder 1.8～2.2: 1 mixing in molar ratio, grind;
Add the excessive Thiovanic acid of deionized water flush away, filter the filter cake deionized water wash;
With filter cake and sodium sulphite 1～3.5: 2 mixing in molar ratio, grind, obtain faint yellow solid;
The faint yellow solid that previous step obtains suddenly is water-soluble, add again in acetone or the ether, make the sedimentation of CdS colloidal sol;
Filter, washing, drying obtains the nano-tube/CdS crystal.
Observe under transmission electron microscope, the particle diameter of nanoparticle is between 3～5nm, and particle distribution is even, no agglomeration.As shown in Figure 1.
Say that more specifically and more optimally method of the present invention is as follows:
In room temperature, under the normal pressure, Thiovanic acid and Cadmium chloride fine powder were mixed in 2: 1 in molar ratio, in mortar, grind, add the excessive Thiovanic acid of deionized water flush away, filter the filter cake deionized water wash.With filter cake and sodium sulphite in molar ratio: mix at 3: 2, in mortar, grind, obtain faint yellow solid, it is water-soluble, add acetone again and make the sedimentation of CdS colloidal sol, filter washing.Vacuum-drying.Obtain the nano-tube/CdS crystal.Observe under transmission electron microscope, the particle diameter of nanoparticle is between 3～5nm, and particle distribution is even, no agglomeration.As shown in Figure 1.
Prioritization scheme of the present invention is: the nano-tube/CdS crystal that above method is obtained is dispersed in the aqueous solution under the ultrasonic wave effect, and the aqueous solution of bovine serum albumin is joined in the aqueous solution of Cadmium Sulfide, and its fluorescence obtains linear the reinforcement, as shown in Figure 2.Linear dependence is 0.9973, as shown in Figure 3.Be expected to it is used as and be biological protein fluorescence probe.
The present invention has the reaction conditions gentleness, and technology is simple, the productive rate height, and the particle diameter of preparation is even, no agglomeration, characteristics such as favorable reproducibility.Because finishing has Thiovanic acid, thereby has solved water-soluble and Bc well.Compare with traditional biological fluorescent labeling (organic dye), the exciting light spectrum width of nanocrystal, and continuous distribution, emmission spectrum be symmetrically distributed and width narrow, color tunable, the optical excitation of nanocrystalline physical efficiency coverlet one wavelength of promptly different sizes and send the light and the photochemical stability height of different colours is difficult for advantages such as photodissociation.The CdS of the present invention's preparation is nanocrystalline owing to solved water-soluble well and Bc, Bovine Serum Albumin in Aqueous Solution is added to makes further in the aqueous solution of CdS colloidal sol that its fluorescence is linear to be strengthened, use it for biological fluorescent labeling, have good development and application prospect.
Description of drawings
Fig. 1 is the transmission electron microscope of the CdS nano material of the present invention's preparation;
Fig. 2 is that the Bovine Serum Albumin in Aqueous Solution with different concns joins in the aqueous solution of Cadmium Sulfide its fluorescence spectrum figure;
Fig. 3 is the linear enhancing figure of fluorescence.
Embodiment
Embodiment 1, and room temperature under the normal pressure, is mixed mixing in 2: 1 in molar ratio with Thiovanic acid and Cadmium chloride fine powder, and milling time 30min in mortar adds the excessive Thiovanic acid of deionized water flush away, filters the filter cake deionized water wash.Filter cake and sodium sulphite were mixed in 3: 2 in molar ratio, in agate mortar, grind, obtain faint yellow solid, it is water-soluble, add acetone again and make the sedimentation of CdS colloidal sol, filter washing.Vacuum-drying.Obtain the nano-tube/CdS crystal.Observe under transmission electron microscope, the particle diameter of nanoparticle is between 3～5nm, and particle distribution is even, no agglomeration.As shown in Figure 1.
Embodiment 2, and is substantially the same manner as Example 1, but Thiovanic acid and Cadmium chloride fine powder blended mol ratio are 1.8: 1; The mol ratio of filter cake and sodium sulphite is 1: 2; The solvent that sedimentation is used is an ether.
Embodiment 3, and is substantially the same manner as Example 1, but Thiovanic acid and Cadmium chloride fine powder blended mol ratio are 2.2: 1; The mol ratio of filter cake and sodium sulphite is 3.5: 2.
Claims (2)
1, the nanocrystalline wet solid state reaction preparation method of a kind of CdS semiconduct may further comprise the steps:
With Thiovanic acid and Cadmium chloride fine powder 1.8～2.2: 1 mixing in molar ratio, grind;
Add the excessive Thiovanic acid of deionized water flush away, filter the filter cake deionized water wash;
With filter cake and sodium sulphite 1～3.5: 2 mixing in molar ratio, grind, obtain faint yellow solid;
The faint yellow solid that previous step obtains suddenly is water-soluble, add again in acetone or the ether, make the sedimentation of CdS colloidal sol;
Filter, washing, drying obtains the nano-tube/CdS crystal.
2, according to the nanocrystalline wet solid state reaction preparation method of the described CdS semiconduct of claim 1, it is characterized in that: mixed in 2: 1 in molar ratio of described Thiovanic acid and Cadmium chloride fine powder, described filter cake and sodium sulphite mixed in 3: 2 in molar ratio;
After the faint yellow solid that obtains was water-soluble, the solvent that is added when making the sedimentation of CdS colloidal sol was an acetone.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410041158 CN1280457C (en) | 2004-07-05 | 2004-07-05 | Wet-solid phase reaction preparation method for cadmium sulfide semiconductor nanocrystalline |
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| CN 200410041158 CN1280457C (en) | 2004-07-05 | 2004-07-05 | Wet-solid phase reaction preparation method for cadmium sulfide semiconductor nanocrystalline |
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| CN1280457C true CN1280457C (en) | 2006-10-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1328157C (en) * | 2006-03-02 | 2007-07-25 | 浙江大学 | Method for preparing non-laminate sulfide nano tube |
| CN101381600B (en) * | 2008-10-22 | 2012-02-01 | 中国科学院上海技术物理研究所 | Preparation method of biocompatible aqueous phase quantum point |
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