CN101941735B - Short rod-like and peony-like lead sulfide nano-structure material and preparation method thereof - Google Patents
Short rod-like and peony-like lead sulfide nano-structure material and preparation method thereof Download PDFInfo
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- CN101941735B CN101941735B CN201010276282XA CN201010276282A CN101941735B CN 101941735 B CN101941735 B CN 101941735B CN 201010276282X A CN201010276282X A CN 201010276282XA CN 201010276282 A CN201010276282 A CN 201010276282A CN 101941735 B CN101941735 B CN 101941735B
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Abstract
The invention a short rod-like and peony-like lead sulfide nano-structure material and a preparation method thereof, belonging to the technical field of nano materials. The preparation method of the short rod-like and peony-like lead sulfide nano-structure material comprises the following steps of: preparing lead sulfide nano materials by directly taking biological nano-structure DNA as a template; sufficiently mixing a DNA solution with the concentration of 1-2mg/mL and a lead nitrate solution with the concentration of 50mM; then carrying out water bath heating to achieve 35-45 DEG C, simultaneously adding a thioacetamide solution with the concentration of 0.4 M, and stirring at low speed; heating to 70 DEG C, and keeping for 5-10 minutes; cooling, then washing and centrifuging to extract sediments, and carrying out drying treatment so as to obtain a lead sulfide nano-structure taking the DNA as the template. The invention directly takes the large biological molecule DNA as the template; the bionic mineralization method has the advantages of easy operation, moderate preparation condition, uniform appearance, can regulate and control the mineral crystal nucleation process through biological molecules, controls the appearance and the structure of a PbS crystal and has unique superiority in the growth research of the PbS crystal.
Description
Technical field
The invention belongs to technical field of nano material, particularly relate to a kind of DNA of utilization biomacromolecule prepares corynebacterium and the flower-shaped lead sulfide nanostructure of tree peony for template technology.
Background technology
Lead sulfide is a kind of cube of rock salt structure semiconductor material, has narrow band gap (0.41eV) and big Bohr's exciton radius (18nm).Sulfide nanocrystalline has strong quantum confined effect; Its cubic non-linearity optical property approximately is 30 times of GaAs; 1000 times of CdSe; At aspects such as near infrared communication, photon switch, heat and bio-imaging, photoelectric device, solar cell and high-efficiency photovoltaic conversions the potential using value is arranged, its tempting application prospect has caused chemist and material supply section scholars' extensive concern and has become the focus of nano materials research.
Preparing method about lead sulfide has much at present.From raw material, roughly be divided into two types: one type is with lead salt (plumbic acetate, lead nitrate, lead perchlorate etc.), and sulfocompound (hydrogen sulfide, thiocarbamide etc.) is made raw material, with micella, and polymkeric substance, molecular sieve or tensio-active agent etc. are controlled synthetic for template.(J.Colloid Interface.2006 is plumbous source, CS with sugar of lead in article 301-503) to people such as Dong in " colloid and interface science "
2For the sulphur source under tensio-active agent cetyl trimethylammonium bromide (CTAB) effect, obtain the PbS nanometer rod after leaving standstill 3d under 40 ℃ of the temperature of reaction, but CS
2Be toxic reagent, human body is had very big toxic action; People such as Wan are at " materials chemistry and materials physics " (Mater.Chem.Phys.2004; 88; 217) assisting through tensio-active agent sodium laurylsulfonate (SDS) in the article; Two-phase interface reaction 20h obtains the PbS nanometer rod under 160 ℃ of conditions, owing to only generating nanometer rod at the interface, its rate ratio is lower.Another kind of is to make raw material through the synthetic lead sulfide nanoparticles of simple substance reaction with simple substance lead, sulphur.(Chem.Commun.1996 uses metallic lead in article 1095-1096) to people such as Parkin, and sulphur is medium with liquefied ammonia, in autoclave, reacts 2～12h and has obtained lead sulfide at " chemical communication ".People such as Zhang Yong are at " the microwave exposure element reaction synthesizes the lead sulfide nanoparticle " (Zhongshan University's journal (natural science edition); 2003,42 (2): 50-51) in this piece article with metallic lead, sulphur and different solvent quadrols, N; A N ' dimethyl methyl phthalein amine; Ammoniacal liquor etc. are reaction medium, and under microwave exposure, elementary sulfur and plumbous single step reaction generate lead sulfide.The shortcoming of these methods is that reaction unit is loaded down with trivial details, and reaction process is comparatively complicated.
Many advantages such as above-mentioned chemical synthesis process condition is relatively harsh, has various defectives, and the biological template method is with its mild condition, and is simple to operate become the research focus of nano structural material in recent years.As (silicate circulates a notice of 2010 in " the biomolecules template prepares different-shape lead sulfide nano material " in people such as saussurea involucrata; 29 (2) 450-457) utilize halfcystine to be template in this piece article; Through controlling its add-on, multiple pattern nanostructures such as dendroid, hierarchy, multi-arm lead sulfide have been synthesized.
Summary of the invention
The objective of the invention is: flower-shaped lead sulfide nano structural material of a kind of corynebacterium and tree peony and preparation method thereof is provided; This method is not only simple to operate; Preparation condition is gentle; Avoided conventional preparing method's complicated technology, and can in the PbS Study on Crystals Growth, have special advantages through the convenient regulation and control ground control PbS crystalline pattern and the structure of biomacromolecule to the mineral crystal nucleation process.
Technical scheme of the present invention is:
Corynebacterium lead sulfide nano structural material is by dna molecular and lead sulfide molecule be combined into, and the length that constitutes the lead sulfide of corynebacterium shape nanostructure is 180～260nm, and diameter is 40～70nm.
Tree peony flower-like nanostructure lead sulfide is by dna molecular and lead sulfide molecule be combined into, and the diameter that constitutes the lead sulfide of tree peony flower-like nanostructure is 800～1400nm.
Method of the present invention is:
Be that template prepares the lead sulfide nano material directly with the biological nano structural DNA; After concentration is the dna solution of 1～2mg/mL and lead nitrate solution thorough mixing that concentration is 50mM; Carry out heating in water bath when arriving 35-45 ℃, adding concentration is the thioacetyl amine aqueous solution of 0.4M, and stirring at low speed; Be heated to 70 ℃ and keep 5-10min, washing after cooling, centrifuging and taking deposition drying treatment are the lead sulfide nanostructure that DNA is a template.
Concrete steps of the present invention are:
(1) be the aqueous dna of 1～2mg/mL and the Pb (NO that concentration is 50mM with concentration
3)
2The aqueous solution is pressed 1: 1 mixed, leaves standstill more than the 24h;
(2) place there-necked flask to its heating in water bath in mixture; Dripping (0.3mL/s) concentration during to 35-45 ℃ is thioacetamide (TAA) aqueous solution of 0.4M; With mixed liquor volume ratio in the step (1) be 1: 2, and stirring at low speed is heated to 70 ℃ and keeps 5-10min;
(3) there-necked flask is cooled to room temperature in the normal temperature water-bath, products therefrom is centrifugal 20～30min under 5000～8000rpm;
(4) centrifugal gained deposition is spent ionized water and anhydrous methanol respectively and wash that can to obtain with DNA after twice ,-45 ℃ of lyophilizes be the corynebacterium and the flower-shaped nanostructure of tree peony of template.
Utilizing DNA is 1～2mg/mL for method used DNA system concentration in step (2) that template prepares corynebacterium and the flower-shaped lead sulfide nanostructure of tree peony, and solution is stored in 4 ℃ of environment, needs mixing repeatedly before using, and DNA is scattered in the deionized water fully.
The invention has the beneficial effects as follows: the notable feature of this method is to be template with biomacromolecule DNA directly, has prepared comparatively special corynebacterium and the flower-shaped nanostructure of tree peony of pattern.This biomimetic mineralization method is simple to operate; Preparation condition is gentle; The pattern homogeneous has overcome conventional preparing method's complicated technology, and can be through the regulation and control of biomolecules to the mineral crystal nucleation process; Control PbS crystalline pattern and structure have special advantages in the PbS Study on Crystals Growth.For the preparation of novel lead sulfide nano material provides practicable thinking, for the regulation and control of further investigation lead sulfide crystal morphology lay the foundation.
Description of drawings
Fig. 1 is to be the SEM figure of the corynebacterium lead sulfide nanostructure of template with DNA;
Fig. 2 is that local that amplify is the SEM figure of the corynebacterium lead sulfide nanostructure of template with DNA;
Fig. 3 is to be the EDS spectrogram of the corynebacterium lead sulfide nanostructure of template with DNA;
Fig. 4 is to be the XRD spectra of the corynebacterium lead sulfide nanostructure of template with DNA;
Fig. 5 is to be the SEM figure of the flower-shaped lead sulfide nanostructure of tree peony of template with DNA, this figure double as Figure of abstract;
That Fig. 6 amplifies the part is the SEM figure of the flower-shaped lead sulfide nanostructure of tree peony of template with DNA;
Fig. 7 is to be the EDS spectrogram of the corynebacterium lead sulfide nanostructure of template with DNA;
Fig. 8 is to be the XRD spectra of the flower-shaped lead sulfide nanostructure of tree peony of template with DNA.
Embodiment
Embodiment 1: the corynebacterium lead sulfide nanostructure preparation that with DNA is template
With 50mL concentration is the aqueous dna of 1mg/mL and the Pb (NO that 50mL concentration is 50mM
3)
2Aqueous solution leaves standstill 24h.Place there-necked flask to its heating in water bath in mixture, dripping (0.3mL/s) 50mL concentration during to 40 ℃ is the TAA aqueous solution of 0.4M, and stirring at low speed, is heated to 70 ℃ and keeps 5min.There-necked flask is cooled to room temperature in the normal temperature water-bath; Products therefrom is centrifugal 20～30min under 5000～8000rpm; Centrifugal gained deposition is spent ionized water and anhydrous methanol respectively wash that can to obtain with DNA after twice ,-45 ℃ of lyophilizes be the corynebacterium nanostructure of template.
Embodiment 2: the flower-shaped lead sulfide nanostructure of the tree peony preparation that with DNA is template
With 50mL concentration is the aqueous dna of 2mg/mL and the Pb (NO that 50mL concentration is 50mM
3)
2Aqueous solution leaves standstill 24h.Place there-necked flask to its heating in water bath in mixture, dripping (0.3mL/s) 50mL concentration during to 40 ℃ is the TAA aqueous solution of 0.4M, and stirring at low speed, is heated to 70 ℃ and keeps 5min.There-necked flask is cooled to room temperature in the normal temperature water-bath; Products therefrom is centrifugal 20～30min under 5000～8000rpm; Centrifugal gained deposition is spent ionized water and anhydrous methanol respectively wash that can to obtain with DNA after twice ,-45 ℃ of lyophilizes be the flower-shaped nanostructure of tree peony of template.
Claims (3)
1. flower-shaped lead sulfide nano structural material of tree peony is characterized in that: by dna molecular and lead sulfide molecule be combined into, the diameter that constitutes the lead sulfide of tree peony flower-like nanostructure is 800～1400nm.
2. the preparation method of the flower-shaped lead sulfide nano structural material of tree peony; Its method is: be that template prepares the lead sulfide nano material with the biological nano structural DNA directly; After concentration is the dna solution of 2mg/mL and lead nitrate solution thorough mixing that concentration is 50mM; Carry out heating in water bath when arriving 35-45 ℃, adding concentration is the thioacetyl amine aqueous solution of 0.4M, and stirring at low speed; Be heated to 70 ℃ and keep 5-10min, washing after cooling, centrifuging and taking deposition drying treatment are the lead sulfide nanostructure that DNA is a template;
A, be the aqueous dna of 2mg/mL and the Pb (NO that concentration is 50mM with concentration
3)
2The aqueous solution mixes by 1: 1 volume ratio, leaves standstill more than the 24h;
B, place there-necked flask to its heating in water bath in mixture, dripping 0.3mL/s concentration during to 35-45 ℃ is the thioacetyl amine aqueous solution of 0.4M, with mixed liquor volume ratio among the step a be 1: 2, and stirring at low speed is heated to 70 ℃ and keeps 5-10min;
C, there-necked flask is cooled to room temperature in the normal temperature water-bath, products therefrom is centrifugal 20～30min under 5000～8000rpm;
D, centrifugal gained deposition spent respectively can to obtain with DNA after ionized water and twice ,-45 ℃ of lyophilizes of anhydrous methanol washing be the flower-shaped nanostructure of tree peony of template.
3. the preparation method of the flower-shaped lead sulfide nano structural material of a kind of tree peony according to claim 2, its method is:
Utilize DNA to be 2mg/mL for method used DNA system concentration in step b that template prepares the flower-shaped lead sulfide nanostructure of tree peony, solution is stored in 4 ℃ of environment, needs mixing repeatedly before using, and DNA is scattered in the deionized water fully.
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| CN102602987B (en) * | 2012-03-08 | 2013-11-20 | 上海交通大学 | Method for preparing protein ribonuclease protein crystal modified lead sulfide nanorod |
| CN102605428A (en) * | 2012-03-16 | 2012-07-25 | 河南大学 | PbS nanomaterial characterized by oriented attachment structure and preparation method thereof |
| CN102674440B (en) * | 2012-05-23 | 2013-12-25 | 许昌学院 | Chemical method for preparing PbS film with peony-shaped surface appearance by ethylenediamine assisted in-situ preparation |
| CN109499517B (en) * | 2018-12-19 | 2022-03-25 | 西北农林科技大学 | Preparation method and application of peony-like SnS nano material |
| CN113621367A (en) * | 2021-06-15 | 2021-11-09 | 哈尔滨理工大学 | Preparation method of rice-grain-shaped lead sulfide quantum dots |
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| KR20060081896A (en) * | 2005-01-10 | 2006-07-14 | 서경식 | Water soluble metal sulfide quantum dot nanocrystal complex |
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