CN104591261B - And preparation method and application of hollow ZnS tetrapod - Google Patents
And preparation method and application of hollow ZnS tetrapod Download PDFInfo
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- CN104591261B CN104591261B CN201410801836.1A CN201410801836A CN104591261B CN 104591261 B CN104591261 B CN 104591261B CN 201410801836 A CN201410801836 A CN 201410801836A CN 104591261 B CN104591261 B CN 104591261B
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- C—CHEMISTRY; METALLURGY
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- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
Abstract
The invention provides a preparation method and application of a hollow ZnS tetrapod. The preparation method comprises the following steps: heating a metal zinc sheet in a pipe furnace, controlling the input of oxygen in a nitrogen protective atmosphere to obtain a ZnO tetrapod, adding the ZnO tetrapod, L-cysteine and Na2S.9H2O into deionized water at room temperature, evenly mixing, heating, cooling to room temperature, filtering, washing and drying to obtain the hollow ZnS tetrapod. The preparation method is simple and can obtain a new-shape ZnS tetrapod; and the ZnS tetrapod can be widely used in the fields of photoinduced fluorescence, fluorescent probes and fluorescent microscopes.
Description
Technical field
The invention belongs to developing material technical field, more particularly to a kind of preparation method and application of hollow ZnS four-footeds body.
Background technology
ZnS is the elementary composition quasiconductor of an II-VI group, and it has very wide energy gap (3.7V), is widely used in light
Cause fluorescence, fluorescent probe and fluorescence microscope[1-6].Physical property of the pattern, size and crystal growth direction of ZnS to it
And application has tremendous influence.Although the various patterns of ZnS, such as nano-particle, nanorod and nanowire[1-6]Deng wide
General prepares and obtains in-depth study, but develops some new patterns, has very for its fluorescence efficiency is improved
Big effect.
The content of the invention
It is an object of the invention to provide a kind of preparation method and application of hollow ZnS four-footeds body, it is desirable to provide Yi Zhongquan
The hollow ZnS four-footeds body of new pattern.
The present invention is achieved in that a kind of preparation method of hollow ZnS four-footeds body, comprises the following steps：
(1) at room temperature, by 0.7～0.9g ZnO four-footed bodies, 0.02～0.04mol L-Cysteine and 2.2～2.6g
Na2S.9H2O is added in 24～26mL deionized waters, is stirred；
(2) after is heated 11～13 hours at 125～135 DEG C the mixture stirred in step (1), naturally cool to
Room temperature, is filtered, washed and dried, and obtains hollow ZnS four-footeds body.
Preferably, in step (1), the amount of the ZnO four-footeds body is 0.8g, and the amount of the L-Cysteine is
0.03mol, the Na2S.9H2The amount of O is 2.4g, and the amount of deionized water is 25ml.
Preferably, in step (2), the mixture is heated 12 hours at 130 DEG C.
Preferably, the ZnO four-footeds body is prepared by the following preparation method：
1) it is placed on metal zinc metal sheet as source metal in a little quartz ampoule, then little quartz ampoule is placed on into big quartz ampoule
Afterbody；
2) big quartz ampoule is placed in tube furnace, wherein, the afterbody of big quartz ampoule is located at the high-temperature region of tube furnace, big quartz
The exit of pipe is located at the low-temperature space of tube furnace, and aluminium-foil paper is placed in big quartz ampoule and between high-temperature region and low-temperature space
At 500 DEG C of warm areas；
3) enter nitrogen quartz ampoule by one and big quartz ampoule afterbody is inserted into by the outlet of big quartz ampoule, by one oxygen quartz is entered
Pipe is inserted in big quartz ampoule and is provided with aluminium-foil paper, and an aerofluxuss quartz ampoule is inserted into into the exit of big quartz ampoule；
4) it is passed through toward in big quartz ampoule after high-purity nitrogen carries out air-discharging 20 minutes by entering nitrogen quartz ampoule, is being kept
On the premise of the flow of nitrogen 600sccm per minute, tube furnace is warming up to high-temperature region with 30 DEG C/min of heating rate
700℃；
5) the flow oxygen of 50sccm is passed through toward in big quartz ampoule by entering oxygen quartz ampoule, after 8 hours, in blanket of nitrogen
Room temperature is naturally cooled under enclosing, the ZnO four-footed bodies of white powder are collected at aluminium-foil paper.
Preferably, in step 4) in, purity ＞ 99.995%, the nitrogen of flow 600sccm are passed through toward in quartz ampoule.
Preferably, in step 5) in, the nitrogen atmosphere be passed through in flow quartz ampoule with 100sccm per minute it is high-purity
Nitrogen.
Invention further provides above-mentioned hollow ZnS four-footeds body is in photoluminescence, fluorescent probe and fluorescence microscope system
The application of standby aspect.
The present invention overcomes the deficiencies in the prior art, there is provided a kind of preparation method of hollow ZnS four-footeds body, by by metallic zinc
Piece is made to be heated in tube furnace, under conditions of nitrogen protection, controls the input of oxygen, ZnO four-footed bodies is obtained, then, in room
Under temperature, by ZnO four-footed bodies, L-Cysteine and Na2S.9H2O is added in deionized water and mixes heating, is cooled to room temperature, passes through
It is filtered, washed and dried, obtains hollow ZnS four-footeds body.
In the present invention, the pattern of ZnO, size and crystal growth direction to the physical property of hollow ZnS four-footeds body and
Using there is tremendous influence.ZnO four-footed bodies with the present invention as template, in the case where L-Cysteine is helped, ZnO and L-Cysteine
Reaction production ZnHS+, then ZnHS+And S2-Reaction production ZnS, while in acid condition, ZnO is very unstable, slowly molten
Solution, finally successfully prepares hollow ZnS four-footeds body.The hollow ZnS four-footeds physical ability is widely used in photoluminescence, fluorescent probe and glimmering
The preparation of light microscope.
Description of the drawings
Fig. 1 is the structural representation of the synthesizer of ZnO four-footeds body of the present invention；Wherein, Figure 1A is the entirety of synthesizer
Structural representation；Figure 1B is the mplifying structure schematic diagram of little quartz ampoule in the synthesizer；
Fig. 2 is the SEM figures of sample in the embodiment of the present invention；Wherein, Fig. 2A is ZnO four-footed bodies；Fig. 2 B are complete ZnS tetra-
Sufficient body；Fig. 2 C are the ZnS four-footed bodies of fracture；
Fig. 3 is the TEM pictures of the sample in differential responses stage in the embodiment of the present invention；Wherein, Fig. 3 A are 0 hour；Fig. 3 B
For 2 hours；Fig. 3 C are 8 hours；Fig. 3 D are 12 hours.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, and
It is not used in the restriction present invention.
The synthesizer of embodiment 1ZnO four-footed body
As shown in figure 1, wherein, Figure 1A is the overall structure diagram of synthesizer；Figure 1B is gravelstone in the synthesizer
The mplifying structure schematic diagram of English pipe.The synthesizer includes tube furnace 1 (stove), big quartz ampoule 2, little quartz ampoule 3, for being input into
Nitrogen enters nitrogen quartz ampoule 4, enters oxygen quartz ampoule 5 for be input into oxygen, for the row for discharging gas in big quartz ampoule 2
Gas quartz ampoule 6, two beakers 7, is respectively arranged with the water of purification gas in beaker 7.
Wherein, metal zinc metal sheet is held in little quartz ampoule 3, then little quartz ampoule 3 is placed on into the afterbody of big quartz ampoule 2, big quartz
The afterbody of pipe 2 is placed in the high-temperature region of tube furnace 1, and the low temperature of tube furnace 1 is then placed at the opening relative with its afterbody of big quartz ampoule 2
Area, tube furnace 1 is heated in high-temperature region, and heat is delivered to low-temperature space by high-temperature region, and keeps after the temperature of high-temperature region, from height
Warm area to low-temperature space is in a thermograde successively decreased.
Masking foil 8 is additionally provided with big quartz ampoule 2, the position that the masking foil 8 is placed should be located at high-temperature region to low-temperature space
Between at 500 DEG C of warm area, oxygen is input in big quartz ampoule 2 by entering oxygen quartz ampoule 5 after water purification in beaker, is entered
Oxygen quartz ampoule 5 is inserted into the position in big quartz ampoule 2 positioned at the lay down location of masking foil 8.Enter nitrogen quartz ampoule 4 from big quartz ampoule 2
Exit be inserted into the afterbody of big quartz ampoule 2.Gas Jing aerofluxuss quartz ampoule 6 in big quartz ampoule 2 is discharged, and is discharged gas and is passed through
After Water warfare in another beaker, finally to airborne release.
In the actual application of the embodiment of the present invention, enter the height that nitrogen to big quartz ampoule 2 is passed through in nitrogen quartz ampoule 4
Warm area, the Zn steam that the high temperature of little quartz ampoule 3 is evaporated is transmitted toward low-temperature space direction, in 500 DEG C of warm areas of big quartz ampoule 2
Place, Zn steam contact with the oxygen that oxygen quartz ampoule 5 is passed through is entered, and generation ZnO four-footed bodies are deposited on tinfoil paper after Zn steam is oxidized
On paper 8.The gas that aerofluxuss quartz ampoule 6 is passed through is discharged, it is ensured that steady air current flows.Additionally, in apparatus of the present invention, arranging little
The purpose of quartz ampoule 3 is load Zn, prevents Zn to be sintered together with big quartz ampoule 2 at high temperature, protects big quartz ampoule 2, together
When also certain control action is pressed with to the steam of Zn.
The preparation of embodiment 2ZnO four-footed body
The synthesizer of the ZnO four-footed bodies in 1 in conjunction with the embodiments, the preparation method of ZnO four-footeds body of the present invention includes following
Step：
1) it is placed on 0.5 gram of metal zinc metal sheet as source metal in a little quartz ampoule 3, then little quartz ampoule 3 is placed on
The afterbody of big quartz ampoule 2；
2) big quartz ampoule 2 is placed in tube furnace 1, wherein, the afterbody of big quartz ampoule 2 is located at the high-temperature region of tube furnace 1, greatly
The exit of quartz ampoule 2 is located at the low-temperature space of tube furnace 1, and aluminium-foil paper 8 is placed in big quartz ampoule 2 and in high-temperature region and low-temperature space
Between 500 DEG C of warm areas at；
3) enter nitrogen quartz ampoule 4 by one and the afterbody of big quartz ampoule 2 is inserted into by the outlet of big quartz ampoule 2, by one oxygen is entered
Quartz ampoule 5 is inserted in big quartz ampoule 2 and is provided with aluminium-foil paper 8, and an aerofluxuss quartz ampoule 6 is inserted into into the outlet of big quartz ampoule 2
Place；
4) nitrogen of purity ＞ 99.995%, flow 600sccm is passed through toward in big quartz ampoule 2 by entering nitrogen quartz ampoule 4
After carrying out air-discharging 20 minutes, on the premise of the flow of nitrogen 600sccm per minute is kept, by tube furnace 1 with 30 DEG C/min
Heating rate high-temperature region is warming up to into 700 DEG C；
5) by entering oxygen quartz ampoule 5 toward the flow oxygen that 50sccm is passed through in big quartz ampoule 2, after 8 hours, per point
Room temperature is naturally cooled under the flow nitrogen atmosphere of clock 100sccm, the ZnO four-footed bodies of white powder are collected at aluminium-foil paper 8.
Embodiment 3
(1) at room temperature, by the 0.7g ZnO four-footed bodies prepared in embodiment 2,0.04mol L-Cysteine and
2.2g Na2S.9H2O is added in 26mL deionized waters, is stirred；
(2) after is heated 11 hours at 135 DEG C the mixture stirred in step (1), room temperature is naturally cooled to, is passed through
It is filtered, washed and dried, obtains hollow ZnS four-footeds body 1.
Embodiment 4
(1) at room temperature, by the 0.9g ZnO four-footed bodies prepared in embodiment 2,0.02mol L-Cysteine and
2.6g Na2S.9H2O is added in 26mL deionized waters, is stirred；
(2) after is heated 13 hours at 125 DEG C the mixture stirred in step (1), room temperature is naturally cooled to, is passed through
It is filtered, washed and dried, obtains hollow ZnS four-footeds body 2.
Embodiment 5
(1) at room temperature, by the 0.8g ZnO four-footed bodies prepared in embodiment 2,0.03mol L-Cysteine and
2.4g Na2S.9H2O is added in 25mL deionized waters, is stirred；
(2) after is heated 12 hours at 130 DEG C the mixture stirred in step (1), room temperature is naturally cooled to, is passed through
It is filtered, washed and dried, obtains hollow ZnS four-footeds body 3.
Effect example
1st, sample characterization
The hollow ZnS four-footeds body 3 prepared with embodiment 5 as this effect example in sample.
The instrument characterized to material has：Scanning electron microscope (SEM) and electron lens (TEM), the instrument of morphology characterization is
Electron scanning Electronic Speculum SEM of JEOL 6700, the accelerating potential of experiment is 5kV.When electron lens is analyzed, nano wire is in ultrasonication
Under be dispersed in ethanol solution, then dispersant liquid drop on carbon film copper mesh；The instrument that electron lens is used is JEOL
2010F, the voltage of operation is 200kV.
2 results and discussion
2.1SEM and TEM
As shown in Fig. 2 Fig. 2A is the pattern of ZnO four-footed bodies before reaction, Fig. 2 B are samples after reaction for the SEM pictures of sample
Pattern.Contrast Fig. 2A and Fig. 2 B, it can be seen that the pattern of four-footed body is not varied widely before and after reaction, after simply reacting
The surface of sample become coarse a bit.Fig. 2 C are the pictures of the four-footed body of a fracture, and a four-footed body rhizopodium therein is
Jing ruptures, but also is parked in side, can certainly, and the fracture of four-footed body is that occur in the sample making course of SEM tests；From disconnected
The four-footed body central point for splitting and the one end for breaking foot, what is can known better finds out, four-footed body sample is hollow after reaction.
In order to further verify that hollow four-foot body is formed during the course of the reaction, the present invention also also carries out TEM to sample
Characterize.Fig. 3 is the TEM pictures of the sample in differential responses stage, and as can be seen from Figure 3A, four-footed body is solid before reaction, and
And surface is smooth；With the carrying out of reaction, the sample surfaces of Fig. 3 B become coarse, but also keep solid state；Reaction continues
Carry out to 8 hours, Fig. 3 C are it has been seen in that the surface formation thin film of four-footed body, defines the structure of cable；Most
Reaction afterwards terminates, and Fig. 3 D are readily apparent that and find out that hollow four-foot body is successfully prepared.
2.2 formation mechenism
As can be seen from the above data, the formation of hollow ZnS four-footeds body is the Na with ZnO four-footed bodies as template2S exists for S sources
ZnO reacts to form ZnS in surface, while ZnO is constantly dissolved the result after removing.Because dissolubility of the ZnO in water is very low, institute
With ZnO and S2-Production ZnS is just relatively difficult for direct reaction.In the present invention, L-Cysteine is introduced
(HSCH2CHNH2COOH), under L-Cysteine help, by reacting (1) and (2), ZnO and S is made2-Reaction production ZnS.Cause
For L-Cysteine and the CH of production2CHNH2COOH+There is certain acidity, in acid condition, ZnO is very unstable, slowly
It is dissolved, finally produces hollow ZnS four-footeds body[7].Correlated response equation is as follows：
3. conclusion
The formation of the hollow ZnS four-footeds body of the present invention be with ZnO four-footed bodies as template, in the case where L-Cysteine is helped, ZnO and
L-Cysteine reaction production ZnHS+, then ZnHS+And S2-Reaction production ZnS, while in acid condition, ZnO is very unstable
It is fixed, slowly it is dissolved, the result for finally obtaining.The hollow ZnS four-footeds physical ability of the present invention is widely used in photoluminescence, fluorescence and visits
Pin and fluorescence microscope field.
List of references：
[1] Yan CL, Xue DF, Room temperature fabrication of hollow ZnS and ZnO
Architectures by a sacrificial template route [J] .J Phys Chem B, 2006,110,14：
7102-7106
[2] Chan W C W, Nie S M.Quantum dot bioconjugates for ultrasensitive
Nonisotopic detection [J] .Science, 1998,281 (5385)：2016-2018.
[3] Larson D R, Zipfel W R.Water-soluble quantum dots for multiphoton
Fluorescence imaging in vivo [J] .Science, 2003,300 (5624)：1434-1436.
[4] Yan CL, Xue DF, General, spontaneous ion replacement reaction for the
Synthesis of micro-and nanostructured metal oxides [J] .J Phys Chem B, 2006,110,
4：1581-1586
[5] Michalet X, Pinaud F F, Bentolila L A, et al.Quantum dots for live
Cells, in vivo imaging, and diagnostics [J] .Science, 2005,307 (5709)：538-544.
[6] Bhargava R N, Gallagher D, Hong X, etal.Optical properties of man-
Gaese-doped nanocrystals of ZnS [J] .Physics Review Letters, 1994,72 (3)：416-419.
[7] Yan CL, Xue DF, Conversion of ZnO Nanorod Arrays into ZnO/ZnS
Nanocable and ZnS Nanotube Arrays via an in Situ Chemistry Strategy[J].J Phys
Chem B, 2006,110：25850-25855
Compared to the shortcoming and defect of prior art, the invention has the advantages that：Preparation method of the present invention is simple,
And a kind of ZnS four-footed bodies of brand-new pattern are obtained, the ZnS four-footed physical abilitys are widely used in photoluminescence, fluorescent probe and glimmering
Light microscope field.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of hollow ZnS four-footeds body, it is characterised in that comprise the following steps：
（1）It is placed on metal zinc metal sheet as source metal in a little quartz ampoule, then little quartz ampoule is placed on into big quartz ampoule
Afterbody；
（2）Big quartz ampoule is placed in tube furnace, wherein, the afterbody of big quartz ampoule is located at the high-temperature region of tube furnace, big quartz ampoule
Exit be located at the low-temperature space of tube furnace, by aluminium-foil paper be placed in big quartz ampoule and between high-temperature region and low-temperature space 500
At DEG C warm area；
（3）Enter nitrogen quartz ampoule by one and big quartz ampoule afterbody is inserted into by the outlet of big quartz ampoule, by one oxygen quartz ampoule is entered
It is inserted in big quartz ampoule and is provided with aluminium-foil paper, an aerofluxuss quartz ampoule is inserted into into the exit of big quartz ampoule；
（4）It is passed through toward in big quartz ampoule after high-purity nitrogen carries out air-discharging 20 minutes by entering nitrogen quartz ampoule, is keeping nitrogen
On the premise of the flow of gas 600sccm per minute, high-temperature region is warming up to into 700 by tube furnace with 30 DEG C/min of heating rate
℃；
（5）The flow oxygen of 50sccm is passed through toward in big quartz ampoule by entering oxygen quartz ampoule, after 8 hours, in nitrogen atmosphere
Under naturally cool to room temperature, at aluminium-foil paper collect white powder ZnO four-footed bodies；
（6）At room temperature, step is taken（5）In obtained ZnO four-footeds 0.7～0.9g of body, 0.02～0.04molL- cysteine and
2.2～2.6gNa2S·9H2O is added in 24～26mL deionized waters, is stirred；
（7）By step（6）In the mixture that stirs after 125～135 DEG C of heating 11～13 hours, naturally cool to room
Temperature, is filtered, washed and dried, and obtains hollow ZnS four-footeds body.
2. the preparation method of hollow ZnS four-footeds body as claimed in claim 1, it is characterised in that described in step (6)
The amount of ZnO four-footed bodies is 0.8g, and the amount of the L-Cysteine is 0.03mol, the Na2S·9H2The amount of O is 2.4g, described
Amount of deionized water is 25ml.
3. the preparation method of hollow ZnS four-footeds body as claimed in claim 1, it is characterised in that described mixed in step (7)
Compound is heated 12 hours at 130 DEG C.
4. the preparation method of hollow ZnS four-footeds body as claimed in claim 1, it is characterised in that in step (4), toward quartz
Purity ＞ 99.995%, the nitrogen of flow 600sccm are passed through in pipe.
5. the preparation method of hollow ZnS four-footeds body as claimed in claim 4, it is characterised in that in step (5), the nitrogen
It is that high-purity nitrogen is passed through in quartz ampoule with the flow of 100sccm per minute that atmosphere is enclosed.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962537A (en) * | 2010-09-16 | 2011-02-02 | 武汉工程大学 | Method for preparing (Zn,Cd)S quantum dot |
| CN103998656A (en) * | 2011-12-07 | 2014-08-20 | 华东理工大学 | Methods of producing cadmium selenide multi-pod nanocrystals |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005194140A (en) * | 2004-01-08 | 2005-07-21 | National Institute For Materials Science | Method of manufacturing zinc sulfide nanocable coated with carbon film and method of manufacturing zinc sulfide nanocable coated with carbon film to which tetrapod like zinc sulfide structure is joined |
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2014
- 2014-12-23 CN CN201410801836.1A patent/CN104591261B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962537A (en) * | 2010-09-16 | 2011-02-02 | 武汉工程大学 | Method for preparing (Zn,Cd)S quantum dot |
| CN103998656A (en) * | 2011-12-07 | 2014-08-20 | 华东理工大学 | Methods of producing cadmium selenide multi-pod nanocrystals |
Non-Patent Citations (3)
| Title |
|---|
| Conversion of ZnO Nanorod Arrays into ZnO/ZnS Nanocable and ZnS Nanotube Arrays via an in Situ Chemistry Strategy;Chenglin Yan et al.;《J. Phys. Chem. B》;20061130;第110卷(第51期);25850-25855 * |
| ZnO Nanotetrapods: Controlled Vapor-Phase Synthesis and Application for Humidity Sensing;Yongfu Qiu et al.;《Adv. Funct. Mater.》;20070412;第17卷;1345-1352 * |
| 以ZnO纳米结构为前驱体制备空心ZnS纳米结构;王辰光 等;《材料导报:研究篇》;20101031;第24卷(第10期);5-7，17 * |
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