CN104591261A - 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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- CN104591261A CN104591261A CN201410801836.1A CN201410801836A CN104591261A CN 104591261 A CN104591261 A CN 104591261A CN 201410801836 A CN201410801836 A CN 201410801836A CN 104591261 A CN104591261 A CN 104591261A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
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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
- C01P2004/03—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, particularly relate to a kind of preparation method and application of hollow ZnS four-footed body.
Background technology
ZnS is the elementary composition semi-conductor of an II-VI group, and it has very wide energy gap (3.7V), is widely used in photoluminescence, fluorescent probe and fluorescent microscope
[1-6].The pattern of ZnS, size and crystal growth direction have tremendous influence to its physical properties and application.Such as, although the various patterns of ZnS, nano particle, nanorod and nanowire
[1-6]deng being prepared widely and obtain deep research, but develop some new patterns, have very large effect for the fluorescence efficiency improving it.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and application of hollow ZnS four-footed body, aim to provide a kind of hollow ZnS four-footed body of brand-new pattern.
The present invention is achieved in that a kind of preparation method of hollow ZnS four-footed body, comprises the following steps:
(1) at room temperature, by 0.7 ~ 0.9g ZnO four-footed body, 0.02 ~ 0.04mol Cys and 2.2 ~ 2.6g Na
2s.9H
2o joins in 24 ~ 26mL deionized water, stirs;
(2) mixture stirred in step (1) after 11 ~ 13 hours, is naturally cooled to room temperature 125 ~ 135 DEG C of heating, through filtering, washing and drying, obtain hollow ZnS four-footed body.
Preferably, in step (1), the amount of described ZnO four-footed body is 0.8g, and the amount of described Cys is 0.03mol, described Na
2s.9H
2the amount of O is 2.4g, and described amount of deionized water is 25ml.
Preferably, in step (2), described mixture was 130 DEG C of heating 12 hours.
Preferably, described ZnO four-footed body is obtained by following preparation method:
1) metal zinc metal sheet is placed in a little silica tube as source metal, less silica tube is placed on the afterbody of large silica tube;
2) large silica tube is placed in tube furnace, wherein, the afterbody of large silica tube is positioned at the high-temperature zone of tube furnace, and the exit of large silica tube is positioned at the cold zone of tube furnace, to be placed in by aluminium-foil paper in large silica tube and 500 DEG C of warm area places between high-temperature zone and cold zone;
3) one is entered nitrogen silica tube to be exported by large silica tube and be inserted into large silica tube afterbody, one is entered oxygen silica tube and be inserted in large silica tube and be provided with aluminium-foil paper place, an exhaust silica tube is inserted into the exit of large silica tube;
4) pass through in large silica tube, to pass into high-purity nitrogen into nitrogen silica tube and carry out air-discharging after 20 minutes, under the prerequisite of flow keeping nitrogen per minute 600sccm, high-temperature zone is warming up to 700 DEG C with the temperature rise rate of 30 DEG C/min by tube furnace;
5) pass through the flow oxygen passing into 50sccm into oxygen silica tube in large silica tube, after 8 hours, naturally cool to room temperature under nitrogen atmosphere, collect the ZnO four-footed body of white powder at aluminium-foil paper place.
Preferably, in step 4) in, in silica tube, pass into the nitrogen of purity > 99.995%, flow 600sccm.
Preferably, in step 5) in, described nitrogen atmosphere is pass into high-purity nitrogen in the flow silica tube with per minute 100sccm.
Invention further provides the application of above-mentioned hollow ZnS four-footed body in prepared by photoluminescence, fluorescent probe and fluorescent microscope.
The present invention overcomes the deficiencies in the prior art, provides a kind of preparation method of hollow ZnS four-footed body, by being done to heat in tube furnace by metal zinc metal sheet; under the condition of nitrogen protection, control the input of oxygen, obtain ZnO four-footed body; then, at room temperature, by ZnO four-footed body, Cys and Na
2s.9H
2o joins mixing heating in deionized water, is cooled to room temperature, through filtering, washing and drying, obtains hollow ZnS four-footed body.
In the present invention, the pattern of ZnO, size and crystal growth direction have tremendous influence to the physical properties of hollow ZnS four-footed body and application.With ZnO four-footed body of the present invention for template, under Cys helps, ZnHS is produced in ZnO and Cys reaction
+, then ZnHS
+and S
2-znS is produced in reaction, and in acid condition, ZnO is very unstable, is slowly dissolved, and finally successfully prepares hollow ZnS four-footed body simultaneously.This hollow ZnS four-footed physical efficiency is widely used in the preparation of photoluminescence, fluorescent probe and fluorescent microscope.
Accompanying drawing explanation
Fig. 1 is the structural representation of the synthesizer of ZnO four-footed body of the present invention; Wherein, Figure 1A is the one-piece construction schematic diagram of synthesizer; Figure 1B is the structure for amplifying schematic diagram of the medium and small silica tube of this synthesizer;
Fig. 2 is the SEM figure of sample in the embodiment of the present invention; Wherein, Fig. 2 A is ZnO four-footed body; Fig. 2 B is complete ZnS four-footed body; Fig. 2 C is the ZnS four-footed body of fracture;
Fig. 3 is the TEM picture of the sample in differential responses stage in the embodiment of the present invention; Wherein, Fig. 3 A is 0 hour; Fig. 3 B is 2 hours; Fig. 3 C is 8 hours; Fig. 3 D is 12 hours.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The synthesizer of embodiment 1ZnO four-footed body
As shown in Figure 1, wherein, Figure 1A is the one-piece construction schematic diagram of synthesizer; Figure 1B is the structure for amplifying schematic diagram of the medium and small silica tube of this synthesizer.This synthesizer comprises tube furnace 1 (stove), large silica tube 2, little silica tube 3, nitrogen silica tube 4 is entered for what input nitrogen, oxygen silica tube 5 is entered for what input oxygen, for exhaust silica tube 6, two beakers 7 of being discharged by gas in large silica tube 2, the water of Purge gas is all housed in beaker 7.
Wherein, metal zinc metal sheet is held in little silica tube 3, again little silica tube 3 is placed on large silica tube 2 afterbody, large silica tube 2 afterbody is placed in the high-temperature zone of tube furnace 1, the opening part that large silica tube 2 is relative with its afterbody is then placed in the cold zone of tube furnace 1, and tube furnace 1 heats in high-temperature zone, and heat is delivered to cold zone by high-temperature zone, and after keeping high-temperature zone temperature, in a thermograde of successively decreasing from high-temperature zone to cold zone.
Masking foil 8 is also provided with in large silica tube 2, this masking foil 8 position of placing should between high-temperature zone to cold zone the warm area place of 500 DEG C, oxygen is input in large silica tube 2 by entering oxygen silica tube 5 after water purification in beaker, enters oxygen silica tube 5 position be inserted in large silica tube 2 and is positioned at masking foil 8 lay down location.Enter nitrogen silica tube 4 is inserted into large silica tube 2 afterbody from the exit of large silica tube 2.Gas in large silica tube 2 through exhaust silica tube 6 discharge, Exhaust Gas after the Water warfare in another beaker, eventually to airborne release.
In the actual application of the embodiment of the present invention, enter in nitrogen silica tube 4 to pass into the high-temperature zone of nitrogen to large silica tube 2, high temperature evaporation Zn steam out in little silica tube 3 is transmitted toward direction, cold zone, at 500 DEG C of warm area places of large silica tube 2, Zn steam with enter the oxygen that oxygen silica tube 5 passes into and contact, the oxidized rear generation ZnO four-footed body of Zn steam is deposited on masking foil 8.The gas passed into discharged by exhaust silica tube 6, and ensure steady air current flowing.In addition, in apparatus of the present invention, the object arranging little silica tube 3 is load Zn, prevents Zn to be at high temperature sintered together with large silica tube 2, protects large silica tube 2, is also pressed with certain control action kou to the steam of Zn simultaneously.
The preparation of embodiment 2ZnO four-footed body
The synthesizer of the ZnO four-footed body in conjunction with the embodiments in 1, the preparation method of ZnO four-footed body of the present invention comprises the following steps:
1) 0.5 gram of metal zinc metal sheet is placed on a little silica tube 3 li as source metal, less silica tube 3 is placed on the afterbody of large silica tube 2;
2) large silica tube 2 is placed in tube furnace 1, wherein, the afterbody of large silica tube 2 is positioned at the high-temperature zone of tube furnace 1, and the exit of large silica tube 2 is positioned at the cold zone of tube furnace 1, to be placed in by aluminium-foil paper 8 in large silica tube 2 and 500 DEG C of warm area places between high-temperature zone and cold zone;
3) one is entered nitrogen silica tube 4 to be exported by large silica tube 2 and be inserted into large silica tube 2 afterbody, one is entered oxygen silica tube 5 and be inserted in large silica tube 2 and be provided with aluminium-foil paper 8 place, an exhaust silica tube 6 is inserted into the exit of large silica tube 2;
4) pass through in large silica tube 2, to pass into purity > 99.995% into nitrogen silica tube 4, the nitrogen of flow 600sccm carries out air-discharging after 20 minutes, under the prerequisite of flow keeping nitrogen per minute 600sccm, high-temperature zone is warming up to 700 DEG C with the temperature rise rate of 30 DEG C/min by tube furnace 1;
5) pass through the flow oxygen passing into 50sccm into oxygen silica tube 5 in large silica tube 2, after 8 hours, under the flow nitrogen atmosphere of per minute 100sccm, naturally cool to room temperature, collect the ZnO four-footed body of white powder at aluminium-foil paper 8 place.
Embodiment 3
(1) the 0.7g ZnO four-footed body, 0.04mol Cys and the 2.2g Na that at room temperature, will prepare in embodiment 2
2s.9H
2o joins in 26mL deionized water, stirs;
(2) mixture stirred in step (1) after 11 hours, is naturally cooled to room temperature 135 DEG C of heating, through filtering, washing and drying, obtain hollow ZnS four-footed body 1.
Embodiment 4
(1) the 0.9g ZnO four-footed body, 0.02mol Cys and the 2.6g Na that at room temperature, will prepare in embodiment 2
2s.9H
2o joins in 26mL deionized water, stirs;
(2) mixture stirred in step (1) after 13 hours, is naturally cooled to room temperature 125 DEG C of heating, through filtering, washing and drying, obtain hollow ZnS four-footed body 2.
Embodiment 5
(1) the 0.8g ZnO four-footed body, 0.03mol Cys and the 2.4g Na that at room temperature, will prepare in embodiment 2
2s.9H
2o joins in 25mL deionized water, stirs;
(2) mixture stirred in step (1) after 12 hours, is naturally cooled to room temperature 130 DEG C of heating, through filtering, washing and drying, obtain hollow ZnS four-footed body 3.
Effect example
1, sample characterization
With the sample that the hollow ZnS four-footed body 3 prepared in embodiment 5 is in this effect example.
Have the instrument that material characterizes: scanning electron microscope (SEM) and electronic lens (TEM), the instrument of morphology characterization is JEOL 6700 electronic scanning Electronic Speculum SEM, and the acceleration voltage of experiment is 5kV.Electronic lens analyze time, nano wire is dispersed in ethanolic soln under ultrasonication, then dispersant liquid drop on carbon film copper mesh; The instrument that electronic lens uses is JEOL 2010F, and the voltage of operation is 200kV.
2 results and discussion
2.1SEM and TEM
As shown in Figure 2, Fig. 2 A is the pattern of ZnO four-footed body before reaction to the SEM picture of sample, and Fig. 2 B is the pattern of sample after reaction.Comparison diagram 2A and Fig. 2 B, can find out that the pattern of four-footed body does not vary widely in the front and back of reaction, just the surface of reacted sample has become coarse a bit.Fig. 2 C is the picture of the four-footed body of a fracture, and a four-footed body rhizopodium wherein ruptures, but also is parked in side, can affirm, the fracture of four-footed body occurs in the sample making course of SEM test; From the four-footed body central point of fracture and one end of disconnected foot, what can know better finds out, after reaction, four-footed body sample is hollow.
In order to verify that hollow four-foot body is formed in reaction process further, the present invention also also carries out TEM sign to sample.Fig. 3 is the TEM picture of the sample in differential responses stage, and as can be seen from Figure 3A, before reaction, four-footed body is solid, and smooth surface; Along with the carrying out of reaction, the sample surfaces of Fig. 3 B becomes coarse, but also keeps solid state; Reaction continues to 8 hours, and Fig. 3 C it has been seen in that the surface of four-footed body forms thin film, defines the structure of cable; Final reaction terminates, and Fig. 3 D has clearly found 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-footed body is with ZnO four-footed body for template, Na
2s is that S source forms ZnS in ZnO surface reaction, and ZnO is constantly dissolved the result after removing simultaneously.Because the solubleness of ZnO in water is very low, so ZnO and S
2-it is just more difficult that direct reaction produces ZnS.In the present invention, Cys (HSCH is introduced
2cHNH
2cOOH), under Cys helps, by reaction (1) and (2), make ZnO and S
2-znS is produced in reaction.Because the CH of Cys and production
2cHNH
2cOOH
+have certain acidity, in acid condition, ZnO is very unstable, has slowly been dissolved, and finally produces hollow ZnS four-footed body
[7].Correlated response equation is as follows:
3. conclusion
The formation of the present invention's hollow ZnS four-footed body is with ZnO four-footed body for template, and under Cys helps, ZnHS is produced in ZnO and Cys reaction
+, then ZnHS
+and S
2-znS is produced in reaction, and in acid condition, ZnO is very unstable, is slowly dissolved, the result finally obtained simultaneously.Hollow ZnS four-footed physical efficiency of the present invention is widely used in photoluminescence, fluorescent probe and fluorescent microscope field.
Reference:
[1]Yan CL，Xue DF，Room temperature fabrication of hollow ZnS and ZnOarchitectures 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 nonisotopicdetection[J].Science，1998，281(5385)：2016-2018.
[3]Larson D R，Zipfel W R.Water-soluble quantum dots for multiphotonfluorescence imaging in vivo[J].Science，2003，300(5624)：1434-1436.
[4]Yan CL，Xue DF，General，spontaneous ion replacement reaction for thesynthesis 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 vivoimaging，and diagnostics[J].Science，2005，307(5709)：538-544.
[6]Bhargava R N，Gallagher D，Hong X，etal.Optical properties of man-gaese-dopednanocrystals of ZnS[J].Physics Review Letters，1994，72(3)：416-419.
[7]Yan CL，Xue DF，Conversion of ZnO Nanorod Arrays into ZnO/ZnS Nanocableand 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 present invention has following beneficial effect: preparation method of the present invention is simple, and obtain a kind of ZnS four-footed body of brand-new pattern, this ZnS four-footed physical efficiency is widely used in photoluminescence, fluorescent probe and fluorescent microscope field.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a preparation method for hollow ZnS four-footed body, is characterized in that, comprise the following steps:
(1) at room temperature, by 0.7 ~ 0.9g ZnO four-footed body, 0.02 ~ 0.04mol Cys and 2.2 ~ 2.6g Na
2s.9H
2o joins in 24 ~ 26mL deionized water, stirs;
(2) mixture stirred in step (1) after 11 ~ 13 hours, is naturally cooled to room temperature 125 ~ 135 DEG C of heating, through filtering, washing and drying, obtain hollow ZnS four-footed body.
2. the preparation method of hollow ZnS four-footed body as claimed in claim 1, is characterized in that, in step (1), the amount of described ZnO four-footed body is 0.8g, and the amount of described Cys is 0.03mol, described Na
2s.9H
2the amount of O is 2.4g, and described amount of deionized water is 25ml.
3. the preparation method of hollow ZnS four-footed body as claimed in claim 1, is characterized in that, in step (2), described mixture was 130 DEG C of heating 12 hours.
4. the preparation method of hollow ZnS four-footed body as claimed in claim 1, is characterized in that, described ZnO four-footed body is obtained by following preparation method:
1) metal zinc metal sheet is placed in a little silica tube as source metal, less silica tube is placed on the afterbody of large silica tube;
2) large silica tube is placed in tube furnace, wherein, the afterbody of large silica tube is positioned at the high-temperature zone of tube furnace, and the exit of large silica tube is positioned at the cold zone of tube furnace, to be placed in by aluminium-foil paper in large silica tube and 500 DEG C of warm area places between high-temperature zone and cold zone;
3) one is entered nitrogen silica tube to be exported by large silica tube and be inserted into large silica tube afterbody, one is entered oxygen silica tube and be inserted in large silica tube and be provided with aluminium-foil paper place, an exhaust silica tube is inserted into the exit of large silica tube;
4) pass through in large silica tube, to pass into high-purity nitrogen into nitrogen silica tube and carry out air-discharging after 20 minutes, under the prerequisite of flow keeping nitrogen per minute 600sccm, high-temperature zone is warming up to 700 DEG C with the temperature rise rate of 30 DEG C/min by tube furnace;
5) pass through the flow oxygen passing into 50sccm into oxygen silica tube in large silica tube, after 8 hours, naturally cool to room temperature under nitrogen atmosphere, collect the ZnO four-footed body of white powder at aluminium-foil paper place.
5. the preparation method of hollow ZnS four-footed body as claimed in claim 4, is characterized in that, in step 4) in, in silica tube, pass into the nitrogen of purity > 99.995%, flow 600sccm.
6. the preparation method of hollow ZnS four-footed body as claimed in claim 5, is characterized in that, in step 5) in, described nitrogen atmosphere is pass into high-purity nitrogen in the flow silica tube with per minute 100sccm.
7. the application of hollow ZnS four-footed body in prepared by photoluminescence, fluorescent probe and fluorescent microscope described in claim 1 or 2.
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Citations (3)
| 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 |
| 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 |
-
2014
- 2014-12-23 CN CN201410801836.1A patent/CN104591261B/en active Active
Patent Citations (3)
| 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 |
| 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 |
|---|
| CHENGLIN YAN ET AL.: "Conversion of ZnO Nanorod Arrays into ZnO/ZnS Nanocable and ZnS Nanotube Arrays via an in Situ Chemistry Strategy", 《J. PHYS. CHEM. B》 * |
| YONGFU QIU ET AL.: "ZnO Nanotetrapods: Controlled Vapor-Phase Synthesis and Application for Humidity Sensing", 《ADV. FUNCT. MATER.》 * |
| 王辰光 等: "以ZnO纳米结构为前驱体制备空心ZnS纳米结构", 《材料导报:研究篇》 * |
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