CN100586863C - Method for controlling micrometre zinc sulphide morphology by Escherichia coli biological template - Google Patents
Method for controlling micrometre zinc sulphide morphology by Escherichia coli biological template Download PDFInfo
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- CN100586863C CN100586863C CN200810079483A CN200810079483A CN100586863C CN 100586863 C CN100586863 C CN 100586863C CN 200810079483 A CN200810079483 A CN 200810079483A CN 200810079483 A CN200810079483 A CN 200810079483A CN 100586863 C CN100586863 C CN 100586863C
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Abstract
The invention relates to a method for controlling micron zinc sulfide shape by an escherichia coli biological template. A micron zinc sulfide material with excellent shape and a short rod-shaped structure is obtained by utilizing the space confinement effect of the biological template, taking the escherichia coli as the biological template, preparing competent cells which incubate with the zinc sulfide system and combine with thermal shock and calcination treatment. The shape control of the zinc sulfide material is carried out by the biological confinement effect existing in nature to obtain the zinc sulfide material with uniform shape and same size, which proves that the biological template can accurately regulate and control the synthesis of the material. The method has the advantages ofsimple process, mild conditions, available materials, low cost and that the obtained material has excellent shape characteristics. In addition, as the biological template has the characteristics of self-breeding and high shape repeatability, and the like, the method can easily realize large-scale production.
Description
Technical field
The present invention relates to a kind of inorganic materials preparing technical field, particularly relate to a kind of method of utilizing Escherichia coli biological template control micrometre zinc sulphide morphology.
Background technology
Metallic sulfide has good electrical property, is widely used in semi-conductor, pigment, photo-luminescent devices, solar cell, infrared detector, fiber optics communication etc.Wherein zinc sulphide is a kind of important luminescent material and semiconductor material, have higher infrared transmittivity and good light, machine, calorifics over-all properties at 3～5 μ m and 8～12 mu m wavebands, being mainly used in numerous areas such as electronic industry, national defense industry, chemical, is one of material that is widely studied and applied in the II-VI compounds of group.Zinc sulphide still is a kind of fluorescence host material of unique properties, has been widely used in the multiple instrument, and as flat-panel monitor, optical excitation diode, solar cell etc.Show and lighting field is widely applied is still micron order macrobead zinc sulphide that in information this mainly is because nano level zinc sulphide defective is more, various defectives interactions have reduced the luminous efficiency of zinc sulfide phosphor.And the particle form of material, the size and the distribution of granularity are very big to the performance impact of zinc sulphide luminescent material.In actual applications, fluorescent material especially the granule-morphology of fluorescent powder material luminescent properties is had crucial meaning.The quality of fluorescent material depends on the uniformity coefficient and the particulate pattern of powder size fully, and the requirement to high-quality fluorescent material is that pattern is even basically, and particle size distribution is narrow.As seen, the excellent properties of ZnS mostly depends on particulate size, distribution and pattern, therefore, how to realize that to the control of its size, size distribution and the modification on pattern and surface be the key of research.The at present existing multiple synthetic method that is used for the zinc sulphide of different purposes has vapor phase process, liquid phase method and solid phase method.The gaseous phase deposition reaction is directly with H
2S gas passes through Zn
2+Carry out precipitin reaction in the solution, the final mean sizes of the may command particles such as pH value, reactant concn and reaction times by changing solution, but the bigger H of reaction needed toxicity
2S gas.The preparation of liquid phase method is various informative, simple to operate, controllable granularity, thereby enjoys attention, and its shortcoming is agglomeration easily to take place cause the pattern irregularity.Room temperature one single-step solid phase reaction need not solvent as a kind of new synthetic method, and the productive rate height is pollution-free, but the product size distribution that obtains is inhomogeneous, the pattern irregularity, and difficulty realizes granular size, the control of pattern.The synthetic method that for this reason needs a kind of brand-new control material pattern is to overcome the above problems.
Summary of the invention
At granule-morphology and the big or small unmanageable problem that the existing method for preparing zinc sulphide exists, the invention provides a kind of method of utilizing Escherichia coli biological template control micrometre zinc sulphide morphology.This invention utilization has the biological structure unit of a dimensioning or pattern as biological template, utilize the space confinement effect of biological template self, form new material or structure by methods such as physics, chemistry according to design requirements, simultaneously biomolecules had improves and strict molecular recognition function can be to the synthetic accuracy controlling of carrying out of material, thus the material that obtains having expected structure and performance.
In order to realize this purpose, the present invention adopts the intestinal bacteria of wide material sources as biological template, big enterobacteria (E.coli) is that Escherichia (Escherichia) is represented bacterium, behave and animal intestinal in often occupy bacterium, generally how not pathogenic, so it is safe and reliable to select for use intestinal bacteria to prepare material as biological template.The about 2 μ m of Bacillus coli cells mean length, the about 0.5 μ m of width is the corynebacterium structure of the little circle in two ends, is the good biological template of corynebacterium micron order structured material.The present invention at first carries out multiplication culture to intestinal bacteria, hypotonic processing, the preparation competent cell, then competent cell and zinc sulphide system are hatched altogether, make the zinc sulphide system stick to the intestinal bacteria surface, handle by thermal shock and impel intestinal bacteria that the zinc sulphide system is sucked in the cell, original position forms the zinc sulphide materials of good corynebacterium pattern under the Escherichia coli biological template effect, remove intestinal bacteria bag quilt through calcination processing, thereby obtain the uniform micrometre zinc sulphide material of pattern.
Technical scheme of the present invention comprises the steps:
(1) intestinal bacteria are inserted in the 50ml LB liquid nutrient medium for preparing in advance, 37 ℃, 120～200r/min shaking table is cultivated 12～20h to make it propagation.Then the intestinal bacteria nutrient solution is placed 10～20min on ice, in 0～6 ℃, the centrifugal 8～15min of 3000～5000r/min gets precipitation.
(2) precipitation is dissolved in the 40ml deionized water, 0～6 ℃, the centrifugal 8～15min of 3000～5000r/min carries out hypotonic, repeats 1～2 time, gets precipitation.
(3) precipitation is dissolved in the Zn (CH of 0.01～0.1M of 40ml precooling
3COO)
22H
2In the O solution, fully mixing is placed 5～15min on ice, and then in 0～6 ℃, the centrifugal 8～15min of 3000～5000r/min gets precipitation.Precipitation is dissolved in again the Zn (CH of 0.01～0.1M of 40ml precooling
3COO)
22H
2In the O solution, fully mixing promptly makes the competent cell suspension.
(4) with 0.091g～0.912g CS (NH
2)
2Join in the competent cell suspension, place 10～30min on ice, in 4 ℃ of refrigerators, leave standstill 20～100h.With above-mentioned solution thermal shock 1～5min in 35～45 ℃ of water-baths, transfer to cooled on ice 1～5min fast then, place 4 ℃ of refrigerators to preserve about 10～40h, at room temperature hatch 10～40h then.
(5) hatched after, solution at the centrifugal 8～15min of 3000～5000r/min, will be precipitated with changing over to behind the 15-25ml dissolved in distilled water in the 50ml teflon-lined still, add the 15-25ml quadrol, heat 15～30h down at 150～300 ℃ then, be chilled to room temperature.With solution centrifugal 8～15min under 2500～4000r/min, get 60～100 ℃ of vacuum-drying 15～40h of precipitation then, promptly get the zinc sulphide materials of corynebacterium pattern.
The present invention directly prepares competent cell with Zn (CH3COO) 22H2O of synthetic ZnS system, both can improve the transformation efficiency of competent cell, does not introduce other element again, to synthetic purer and the uniform ZnS of pattern is significant.When intestinal bacteria after hatching altogether of calcining and ZnS system, add and have alkaline quadrol, can more easily dissolve intestinal bacteria bag quilt, meanwhile, the temperature when also reducing calcining just can realize removing the effect that intestinal bacteria are wrapped quilt under lower temperature.
The invention has the beneficial effects as follows: by the space confinement effect of biological template self, adopt the Escherichia coli biological template of wide material sources, hatch and combine thermal shock and calcination processing altogether through the preparation competent cell and with material system, obtain the superior corynebacterium structure micrometre zinc sulphide material of pattern.Owing to colibacillary protection and space confinement effect, can obviously improve the pattern and the stability of material.The zinc sulphide materials pattern that obtains is even, and size is consistent, shows that biological template has accurate control action kou to material synthetic.The inventive method technology is simple, mild condition, and environment-friendly high-efficiency, and raw material sources extensively are easy to get, with low cost, be easy to realize scale operation, the material that is obtained also has good shape characteristic, can be used as the substrate material of high-quality fluorescent material, be widely used, be of great immediate significance.
Description of drawings
The invention will be further elaborated below in conjunction with description of drawings and embodiment.
Fig. 1 carries out the colibacillary TEM figure in hypotonic back;
Fig. 2 is the TEM figure after competent cell and ZnS material system are hatched altogether;
Fig. 3 is resulting a plurality of corynebacterium micrometre zinc sulphide particulate TEM figure after the calcination processing;
Fig. 4 is the EDS figure of the corynebacterium zns particle for preparing of the present invention;
Fig. 5 is the PL figure of the corynebacterium zns particle for preparing of the present invention.
Embodiment
Embodiment 1
Preparation LB liquid nutrient medium 50ml introduces the intestinal bacteria bacterial classification, cultivates 12h at 37 ℃ of following 200r/min shaking tables.Then the intestinal bacteria nutrient solution is placed 10min on ice, at 6 ℃, 3000r/min centrifugation 15min, abandoning supernatant is dissolved in precipitation in the 40ml deionized water, and 6 ℃, the centrifugal 15min of 3000r/min carries out hypotonic, repeats once to get precipitation.Precipitation is dissolved in 40ml, the Zn (CH of 0.01mol/L
3COO)
22H
2In the O solution (precooling in 4 ℃ of refrigerators), fully mixing leaves standstill 5min on ice, and in 6 ℃, 3000r/min centrifugation 15min gets precipitation.Precipitation is dissolved in again the Zn (CH of the 0.01mol/L of 40ml precooling
3COO)
22H
2In the O solution, fully mixing makes competent cell.Take by weighing the CS (NH of 0.091g
2)
2Join in the competent cell suspension, place 10min on ice, after 4 ℃ of refrigerators left standstill 20h, thermal shock 1min in 35 ℃ hot water bath transferred to cooled on ice 1min fast, after preserve about 10h in 4 ℃ of refrigerators again, at room temperature continue to hatch 10h then.The hatching back will be precipitated with changing over to behind the 15ml dissolved in distilled water in the 50ml teflon-lined still at the centrifugal 15min of 3000r/min, add the 25ml quadrol, heat 15h down at 300 ℃ then, be chilled to room temperature.Then with solution at the centrifugal 15min of 2500r/min, be deposited in 100 ℃ of following vacuum-drying 15h, promptly get the micrometre zinc sulphide material of corynebacterium pattern.
Embodiment 2
Preparation LB liquid nutrient medium 50ml introduces the intestinal bacteria bacterial classification, cultivates 17h at 37 ℃ of following 150r/min shaking tables.Then the intestinal bacteria nutrient solution is placed 10min on ice, at 4 ℃, 4000r/min centrifugation 10min, abandoning supernatant is dissolved in precipitation in the 40ml deionized water, and 4 ℃, the centrifugal 10min of 4000r/min carries out hypotonic, repeats twice, gets precipitation.Precipitation is dissolved in 40ml, the Zn (CH of 0.1mol/L
3COO)
22H
2In the O solution (precooling in 4 ℃ of refrigerators), fully mixing leaves standstill 10min on ice, and in 4 ℃, 4000r/min centrifugation 10min gets precipitation.Precipitation is dissolved in again the Zn (CH of the 0.1mol/L of 40ml precooling
3COO)
22H
2In the O solution, fully mixing makes competent cell.Take by weighing the CS (NH of 0.912g
2)
2Join in the competent cell suspension, place 20min on ice, after 4 ℃ of refrigerators left standstill 40h, thermal shock 3min in 42 ℃ hot water bath transferred to cooled on ice 5min fast, after preserve about 10h in 4 ℃ of refrigerators again, at room temperature continue to hatch 22h then.The hatching back will be precipitated with changing over to behind the 20ml dissolved in distilled water in the 50ml teflon-lined still at the centrifugal 10min of 3000r/min, add the 20ml quadrol, heat 22h down at 180 ℃ then, be chilled to room temperature.Then with solution at the centrifugal 10min of 3000r/min, be deposited in 80 ℃ of following vacuum-drying 22h, promptly get the micrometre zinc sulphide material of corynebacterium pattern.
Embodiment 3
Preparation LB liquid nutrient medium 50ml introduces the intestinal bacteria bacterial classification, cultivates 20h at 37 ℃ of following 120r/min shaking tables.Then the intestinal bacteria nutrient solution is placed 20min on ice, at 0 ℃, 5000r/min centrifugation 8min, abandoning supernatant is dissolved in precipitation in the 40ml deionized water, and 0 ℃, the centrifugal 8min of 5000r/min carries out hypotonic, repeats twice, gets precipitation.Precipitation is dissolved in 40ml, the Zn (CH of 0.1mol/L
3COO)
22H
2In the O solution (precooling in 4 ℃ of refrigerators), fully mixing leaves standstill 15min on ice, and in 0 ℃, 5000r/min centrifugation 8min gets precipitation.Precipitation is dissolved in again the Zn (CH of the 0.1mol/L of 40ml precooling
3COO)
22H
2In the O solution, fully mixing makes competent cell.Take by weighing the CS (NH of 0.912g
2)
2Join in the competent cell suspension, place 30min on ice, after 4 ℃ of refrigerators left standstill 100h, thermal shock 5min in 45 ℃ hot water bath transferred to cooled on ice 5min fast, after preserve about 40h in 4 ℃ of refrigerators again, at room temperature continue to hatch 40h then.The hatching back will be precipitated with changing over to behind the 25ml dissolved in distilled water in the 50ml volumetrical teflon-lined still at the centrifugal 8min of 5000r/min, add the 15ml quadrol, heat 30h down at 150 ℃ then, be chilled to room temperature.Then with solution at the centrifugal 8min of 4000r/min, be deposited in 60 ℃ of following vacuum-drying 40h, promptly get the micrometre zinc sulphide material of corynebacterium pattern.
Fig. 1 is the colibacillary TEM figure in hypotonic back, as can be seen from the figure, the intestinal bacteria after hypotonic are swelling state, and the material of cell walls inside owing to be subjected to the osmotic pressure effect part ooze out, the hypotonic repeatedly internal medium that can cause hollow several times helps entering of extraneous reaction system.
Fig. 2 is the TEM figure after competent cell and ZnS material system are hatched altogether, can find out obviously that from figure the ZnS system enters into intestinal bacteria inside, the pattern rule, and size is even, and transformation efficiency is very high.Can see that from the illustration in the lower left corner hollow intestinal bacteria that do not enter ZnS form tangible contrast with the intestinal bacteria that are full of ZnS.
Shown in Fig. 3 is representational a plurality of corynebacterium micrometre zinc sulphide particulate TEM figure, after removing colibacillary bag quilt through calcining as we can see from the figure, ZnS granule-morphology rule, be the corynebacterium particle, and size evenly, the about 0.5 μ m of width average, the about 0.8 μ m of mean length shows that biological template has certain control action kou really to the pattern of material.
Fig. 4 is the EDS figure of the corynebacterium zns particle for preparing of the present invention, from seeing by spectrogram, the corynebacterium zinc sulphide that we prepare is elementary composition by Zn and two kinds of S, the Cu peak is owing to make due to the substrate of copper mesh among the figure, do not have other impurity components, hence one can see that, and sample is quite purified ZnS, the per-cent of Zn atom and S atom is respectively 29.59 and 56.83, and promptly resulting zinc sulphide materials is a non-stoichiometric.
Fig. 5 is the photoluminescence spectrogram of the corynebacterium zns particle for preparing of the present invention, and exciting light wavelength is 320nm, from fluorescence spectrum figure as can be seen sample two tangible glow peaks are arranged, lay respectively at 360nm and 467nm.It is generally acknowledged that the emission peak that is positioned at 400～500nm interval is caused by surface imperfection, so the luminous zone of 467nm is by due to the surface imperfection, it is luminous to be by Zn
2+The room forms.As we can see from the figure, the luminous zone of 467nm a little less than, as seen utilize the surface and the interfacial effect of the corynebacterium ZnS particle that Escherichia coli biological template obtains to cause its surface imperfection littler than previous methods, thus a little less than causing its defective emissive porwer.Hyeon seminar (Hyeon, J.Am.Chem.Soc. such as T., 2005,127:5662) the report band edge that is of a size of the ZnS nanoparticle about 5nm is transmitted near the 335nm, and when size increased, its band edge was launched red shift and is followed to a certain degree broadening phenomenon.In conjunction with former research results, can think the nearly band edge emission of ZnS with being positioned at emission peak about 360nm, compare with report, emission peak peak position generation red shift, its reason may be that the ZnS grain fineness number increases because the ZnS of preparation is of a size of micron order, and energy gap reduces, width between each defect level is also reducing, and therefore the light of emission moves to low frequency.In the prepared in this experiment zinc sulphide sample, be to have regular rod-short pattern with the difference that prepared the spheroidal particle maximum in the past, this difference can cause the difference of zinc sulphide surface state, and then causes the difference of photoluminescence performance.This shows, the influence that utilizes intestinal bacteria can not produce essence to the fluorescence property of ZnS as biological template, it mainly acts on granularity and the pattern that also is to control ZnS, thereby obtains required fluorescence property.
Claims (1)
1. method of utilizing Escherichia coli biological template control micrometre zinc sulphide morphology, it is characterized in that: described method comprises the steps:
(1) intestinal bacteria are inserted in the 50ml LB liquid nutrient medium for preparing in advance, 37 ℃, 120～200r/min shaking table is cultivated 12～20h to make it propagation; Then the intestinal bacteria nutrient solution is placed 10～20min on ice, in 0～6 ℃, the centrifugal 8～15min of 3000～5000r/min gets precipitation;
(2) precipitation is dissolved in the 40ml deionized water, 0～6 ℃, the centrifugal 8～15min of 3000～5000r/min carries out hypotonic, repeats 1～2 time, gets precipitation;
(3) precipitation is dissolved in the Zn (CH of 0.01～0.1M of 40ml precooling
3COO)
22H
2In the O solution, fully mixing is placed 5～15min on ice, and then in 0～6 ℃, the centrifugal 8～15min of 3000～5000r/min gets precipitation; Precipitation is dissolved in again the Zn (CH of 0.01～0.1M of 10ml precooling
3COO)
22H
2In the O solution, fully mixing promptly makes the competent cell suspension;
(4) with 0.091g～0.912g CS (NH
2)
2Join in the competent cell suspension, place 10～30min on ice, in 4 ℃ of refrigerators, leave standstill 20～100h; With above-mentioned solution thermal shock 1～5min in 35～45 ℃ of water-baths, transfer to cooled on ice 1～5min fast then, place 4 ℃ of refrigerators to preserve 10～40h, at room temperature hatch 10～40h then;
(5) hatched after, solution at the centrifugal 8～15min of 3000～5000r/min, will be precipitated with changing over to behind the 15-25ml dissolved in distilled water in the 50ml volumetrical teflon-lined still, add the 15-25ml quadrol, heat 15～30h down at 150～300 ℃ then, be chilled to room temperature; With solution centrifugal 8～15min under 2500～4000r/min, get 60～100 ℃ of vacuum-drying 15～40h of precipitation then, promptly get the zinc sulphide materials of corynebacterium pattern.
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| CN101805022B (en) * | 2010-04-28 | 2011-11-16 | 燕山大学 | Method for preparing barium tungstate nanometer double-line arrays by using DNA as templates |
| CN101880055B (en) * | 2010-07-01 | 2012-05-30 | 燕山大学 | Method for controlling synthesis of starfish-shaped nano-zinc sulfide by utilizing oligo DNA biological template |
| CN102249401B (en) * | 2011-04-06 | 2012-09-26 | 长安大学 | Preparation method of multipurpose compound photocatalytic biological cell vector |
| CN102872775A (en) * | 2012-10-16 | 2013-01-16 | 湖南大学 | Method for preparing hollow material |
| CN105174302B (en) * | 2015-09-21 | 2017-01-25 | 陕西科技大学 | Red low-angle-dependence zinc sulfide structure color materials and preparation method thereof |
| CN106362151B (en) * | 2016-10-26 | 2019-05-28 | 燕山大学 | A kind of preparation method of Escherichia coli@magnetic particle magnetic target medicine carrier |
| CN109205658B (en) * | 2018-10-25 | 2019-04-26 | 北京航空航天大学 | The method of Escherichia coli template contral cadmium sulfide size and shape |
| CN110104673B (en) * | 2019-04-26 | 2021-07-20 | 西北工业大学 | Method for preparing nano zinc oxide based on lactobacillus casei secretion |
| CN114082979B (en) * | 2021-11-15 | 2023-05-26 | 华侨大学 | Carbon material with high monoatomic load, preparation method and application thereof |
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