CN1235808C - Method for preparing zine sulfide nanometer material with orientation arrangement nano-tubes - Google Patents
Method for preparing zine sulfide nanometer material with orientation arrangement nano-tubes Download PDFInfo
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- CN1235808C CN1235808C CN 200410015985 CN200410015985A CN1235808C CN 1235808 C CN1235808 C CN 1235808C CN 200410015985 CN200410015985 CN 200410015985 CN 200410015985 A CN200410015985 A CN 200410015985A CN 1235808 C CN1235808 C CN 1235808C
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Abstract
The present invention relates to a preparation method for a zinc sulfide nanometer material with nanometer tubes arranged in an oriented mode. A zinc oxide nanometer material with nanometer rods arranged in an oriented mode is prepared by a chemical solution method firstly; then, one-dimensional zinc oxide crystals are sulfurized by the chemical solution method and are arranged. In a tetrafluoroethylene container, sulfur sources are dissolved in a solvent according to a certain concentration and are stirred to the state that a solution is clear; then, the zinc oxide material with nanometer rods, which are prepared in advance, are immersed in a reaction solution in the vertical direction; the temperature of the reaction solution rises to 130 DEG C, and the reaction solution reacts for 47 to 49 hours; thus, the zinc sulfide nanometer material with nanometer tubes arranged in an oriented mode can be obtained; the average particle diameter of the crystals is 100 nanometers. The preparation method of the present invention has the advantages of simple operation, low cost and high efficiency, and can realize large area transmission from the zinc oxide nanometer material with nanometer rods arranged in an oriented mode to the zinc sulfide nanometer material with nanometer tubes arranged in an oriented mode. The prepared zinc sulfide nanometer material has good fluorescence performance.
Description
Technical field
The present invention relates to a kind of preparation method of zinc sulfide nano-material, relate in particular to the preparation method of the zinc sulfide nano-material that a kind of nanotube aligns, adopt the chemical solution growth method to prepare the zinc sulfide nano-material that nanotube aligns.
Background technology
Development along with nanotechnology, the technology of preparing of nano material is more and more abundanter, comprises chemical vapor deposition (CVD), magnetron sputtering method, spray pyrolysis, pulsed laser deposition (PLD), atomic-layer epitaxial growth method, molecular beam epitaxy, sol-gel method, hydrolysis method, hydrothermal method, antiphase emulsifiable method, the precipitator method and electrochemical deposition method or the like.Yet the technology of preparing of nano material and the physics of itself, chemical property have much relations.Can prepare by the method for gas phases such as high temperature oxidation mostly such as oxide compound, yet many structural metals sulphur, selenium compound but are difficult to synthesize with this method.Therefore, utilize a kind of technology that oxide compound is transformed into sulfide, the novel nano-material of preparing desired structure is significant for the performance of range of application that enlarges nano material and research novel texture nano material.
Zinc sulphide is a kind of good semiconductor material.When the energy gap of zinc sulphide reached 3.6eV.0K, the band gap of its body material was 325nm; Because the thermal equilibrium phonon is filled, its effective band gap is about 339nm during 300K.It has piezoelectricity and thermoelectric property, and is the optical conductor with 340nm maximum wavelength.Solid-state ZnS is penetrated by ultraviolet radiation (being lower than 335nm), negative electrode to open, X ray, gamma-rays and electric field (electroluminescence) produce radiation when exciting, and is a kind of good fluorescent material.In addition, nanometer along with semiconductor material, can not only cause absorbing wavelength and fluorescent emission generation blue shift, can also produce the optical nonlinearity response, and the redox ability of enhancing nanoparticle, have more excellent photoelectric catalytically active, will be used widely at aspects such as luminescent material, nonlinear optical material, photocatalyst materials.Because these excellent performances of nano-zinc sulfide and potential using value, the nano-zinc sulfide powder body material is preparing by the several different methods success.Yet the assembling on certain substrate (such as silicon chip) of the application need nano material of nano material is lined up and just can be made its concrete being applied on the corresponding nano functional device by it being carried out graphically wait processing.At present, the preparation of having only the minority bibliographical information to arrange about the zinc sulfide nano crystal of different structure, and also these methods only are confined to gas phase synthesis method.Because gas phase synthesis method needs complex apparatus, higher preparation temperature, harsh reaction atmosphere shortcomings such as (high vacuum, protection of inert gas) aspect the large-scale application of material significant limitation being arranged.Under comparing, the chemical solution synthesis method has that equipment is simple, temperature of reaction is low, cost is low, the efficient advantages of higher, and the preparation that is used for the zinc sulphide powder material of success, yet this method also is not used for the preparation that the zinc sulfide nano structured material is arranged by the exploitation of success at present.Therefore, it is significant for the application of this material to find a kind of preparation to have the chemical solution method of arrangement architecture zinc sulphide.
Under comparing, the successful method of passing through gas phase, liquid phase of nano zinc oxide material with big area arrangement architecture prepares.Be sulfided into zinc sulfide nano-material if adopt certain method will have the arrangement architecture nano zinc oxide material, will have huge pushing effect the application of zinc sulfide nano-material with arrangement architecture.2003, the Nano Letter magazine of American Chemical Society was delivered about zinc oxide nano rod and has been arranged the sulfurized article, had opened up the new direction of the zinc sulfide nano-material that the preparation nanotube aligns.Yet, the preparation method that this report adopts (referring to sulfuration) is a high-temperature gas sulfuration method, the zinc oxide nano-crystal arrangement material that soon prepares is in advance put into the steam of hydrogen sulfide or elemental sulfur, preparation zinc sulfide nano pipe under 500～600 degrees centigrade of reactions.This method needs severe condition such as high temperature is airtight, realizes difficulty, cost is high, controllability is low.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, the preparation method of the zinc sulfide nano-material that a kind of nanotube aligns is provided, simple to operate, cost is low, the efficient height, and environmental pollution is little.
For realizing such purpose, in the technical scheme of the present invention, at first adopt chemical solution method to prepare the nano zinc oxide material that aligns, the nano zinc oxide material that adopts chemical solution method sulfuration nanometer rod to align then.In the tetrafluoroethylene container, the sulphur source is dissolved in the solvent according to certain concentration, is stirred to the solution clarification.Be immersed in the reaction soln with certain angle behind the zinc-oxide film that the nanometer rod that will prepare is in advance again arranged, be warming up to 130 ℃, reaction can obtain the zinc sulfide nano-material of tubular arrangement structure in 47-49 hour.Nanotube in the material is to be made of zinc sulfide nano crystal, and the crystalline median size is 100 nanometers.
Preparation method of the present invention comprises following concrete steps:
1. the preparation of the nano zinc oxide material that aligns of nanometer rod:
A) preparation of chemically grown reaction solution: zinc salt, thiocarbamide, ammoniacal liquor and ammonium salt are dissolved in deionized water by a certain percentage, be prepared into the film growth reaction solution, contain zinc salt 0.01mol, 25% (mass ratio) ammoniacal liquor 5ml, thiocarbamide 0.01mol and ammonium salt 0.002mol in every 100ml reaction solution;
The said zinc salt of the present invention is a zinc nitrate hexahydrate; Ammonium salt is an ammonium chloride.
B) pre-treatment of substrate: at first quartz substrate was immersed in the vitriol oil of ebullient 98% 5～10 hours, was immersed in then in the acetone ultrasonic 30～60 minutes, next use a large amount of deionized water rinsings, at last substrate is dried in vacuum drying oven, stand-by.
C) nano zinc oxide material that aligns of nanometer rod is synthetic: before reaction, at first substrate is soaked in the above-mentioned chemically grown reaction soln for preparing; Reaction system is warming up to 94～97 ℃ again, temperature rise rate 10～20 degree/minute, reacted 45～60 minutes down at 94～97 ℃.Reaction finishes the back cools off fast with frozen water, substrate is put in deionized water for ultrasonic 1～2 minute then, uses a large amount of deionized water rinsings, can obtain the nano zinc oxide material that nanometer rod aligns through drying naturally after repeatedly washing.
2. synthetic (sulfuration of zinc oxide) of the zinc sulfide nano-material that aligns of nanotube:
A) preparation of vulcanization reaction solution: the sulphur source is dissolved in the deionized water, is stirred to the solution clarification, can be prepared into vulcanization reaction solution.Wherein the concentration in sulphur source is 1.5 grams/100 ml waters.
B) synthetic (sulfuration of zinc oxide) of the zinc sulfide nano-material that aligns of nanotube: the zinc oxide nano film that will prepare in advance vertically is immersed in the above-mentioned vulcanization reaction solution for preparing, closed reaction vessel, pack in the stainless steel cauldron, be warming up to 130 ℃, reacted 47-49 hour, reaction naturally cools to normal temperature after finishing, and takes out the sample deionized water rinsing, can obtain the zinc sulfide nano-material that nanotube aligns through drying naturally after repeatedly washing.Nanotube crystalline median size is 100 nanometers in the material.
The said sulphur of the present invention source is a thioacetamide.
The chemical solution method temperature of reaction that the present invention adopts is low, only needs 130 ℃, and aqueous solvent is prevailing solvent, cost is low, pollution is little, helps environmental protection, thereby the inventive method is simple to operate, cost is low, the efficient height, the matrix material of preparing has good fluorescence property.Adopt method of the present invention, can realize that the big area of the zinc sulfide nano-material that the nano zinc oxide material that aligns from nanometer rod aligns to nanotube transforms.
Description of drawings
The x-ray diffraction pattern of the nano zinc oxide material that the nanometer rod that Fig. 1 is adopted for the embodiment of the invention 1 aligns.
The x-ray diffraction pattern of the zinc sulfide nano-material that Fig. 2 aligns for the embodiment of the invention 1 resulting nanotube.
The electron scanning micrograph of the nano zinc oxide material that the nanometer rod that Fig. 3 is adopted for the embodiment of the invention 1 aligns.
The electron scanning micrograph of the zinc sulfide nano-material that Fig. 4 aligns for the embodiment of the invention 1 resulting nanotube.
The scanning electronic microscope enlarged photograph of the zinc sulfide nano-material that Fig. 5 aligns for the embodiment of the invention 1 resulting nanotube.
The transmission electron microscope photo that the zinc sulfide nano-material that Fig. 6 aligns for the embodiment of the invention 1 resulting nanotube is arranged.
The fluorescence spectrum figure of the zinc sulfide nano-material that Fig. 7 aligns for the embodiment of the invention 1 resulting nanotube.
Embodiment
The following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1
1. the preparation of the nano zinc oxide material that aligns of nanometer rod:
A) preparation of chemically grown reaction solution: zinc nitrate hexahydrate, thiocarbamide, ammoniacal liquor and ammonium chloride are dissolved in deionized water by a certain percentage, be prepared into the film growth reaction solution, contain zinc nitrate hexahydrate 0.01mol, 25% (mass ratio) ammoniacal liquor 5ml, thiocarbamide 0.01mol and ammonium chloride 0.002mol in every 100ml aqueous solution;
B) pre-treatment of substrate: at first quartz substrate was immersed in the vitriol oil of ebullient 98% 10 hours, was immersed in then in the acetone ultrasonic 60 minutes, next use a large amount of deionized water rinsings, at last substrate is dried in vacuum drying oven, stand-by.
C) nano zinc oxide material that aligns of nanometer rod is synthetic: before reaction, at first substrate is soaked in the above-mentioned chemically grown reaction soln for preparing; Reaction system is warming up to 95 ℃ again, temperature rise rate 15 degree/minute, reacted 60 minutes down at 95 ℃.Reaction finishes the back cools off fast with frozen water, substrate is put in deionized water for ultrasonic 1 minute then, uses a large amount of deionized water rinsings, can obtain the nano zinc oxide material that nanometer rod aligns through drying naturally after repeatedly washing.
2. synthetic (sulfuration of zinc oxide) of zinc sulfide nano pipe:
A) preparation of vulcanization reaction solution: 3 gram thioacetamides according to being dissolved in 200 ml deionized water, are stirred to the solution clarification, can be prepared into vulcanization reaction solution.
B) synthetic (sulfuration of zinc oxide) of the zinc sulfide nano-material that aligns of nanotube: from the above-mentioned vulcanization reaction solution for preparing, take out 30 milliliters, pour in 40 milliliters the tetrafluoroethylene inner bag, the zinc oxide nano film for preparing in advance vertically is immersed in the vulcanization reaction solution, airtight water heater container, pack in the stainless steel cauldron, be warming up to 130 ℃, reacted 48 hours, reaction naturally cools to normal temperature after finishing, take out the sample deionized water rinsing, can obtain the zinc sulfide nano-material that nanotube aligns through drying naturally after repeatedly washing.
X-ray diffraction spectrogram such as Fig. 1 of the zinc-oxide film that adopts, prepared as seen from Figure 1 zinc oxide are hexagonal crystal shape (36-1451), and strength ratio [101] crystal face of crystal face [002] is a lot of by force, illustrate that zincite crystal is along good orientation is axially arranged.The x-ray diffraction pattern of the zinc sulfide nano-material that resulting nanotube aligns such as Fig. 2, prepared as seen from Figure 2 nanotube is arranged as single zinc sulfide crystal.The electron scanning micrograph of the nano zinc oxide material that the nanometer rod that is adopted aligns such as Fig. 3, prepared as seen from Figure 3 zinc oxide are the one-dimensional rod-like crystal, and these crystal are along axially be arranged in thin-film material on quartz substrate.Electron scanning micrograph such as Fig. 4 and Fig. 5 of the zinc sulfide nano-material that the resulting nanotube in sulfuration back aligns, visible nanotube is made of particle grain size average out to 100 nanometers granular small-crystalline.Fig. 6 is resulting zinc sulfide nano pipe electronic scanning electromicroscopic photograph, and viewed pattern is consistent with scanning electron microscope.Fig. 7 is the fluorescence spectrum figure of resulting zinc sulfide nano pipe.As seen from Figure 7, the zinc sulfide nano-material that aligns of prepared nanotube has fluorescent effect.
Embodiment 2
1. the preparation of the nano zinc oxide material that aligns of nanometer rod:
A) preparation of chemically grown reaction solution: zinc nitrate hexahydrate, thiocarbamide, ammoniacal liquor and ammonium chloride are dissolved in deionized water by a certain percentage, be prepared into the film growth reaction solution, contain zinc nitrate hexahydrate 0.01mol, 25% (mass ratio) ammoniacal liquor 5ml, thiocarbamide 0.01mol and ammonium chloride 0.002mol in every 100ml aqueous solution;
B) pre-treatment of substrate: at first quartz substrate was immersed in the vitriol oil of ebullient 98% 10 hours, was immersed in then in the acetone ultrasonic 60 minutes, next use a large amount of deionized water rinsings, at last substrate is dried in vacuum drying oven, stand-by.
C) nano zinc oxide material that aligns of nanometer rod is synthetic: before reaction, at first substrate is soaked in the above-mentioned chemically grown reaction soln for preparing; Reaction system is warming up to 95 ℃ again, temperature rise rate 15 degree/minute, reacted 60 minutes down at 95 ℃.Reaction finishes the back cools off fast with frozen water, substrate is put in deionized water for ultrasonic 1 minute then, uses a large amount of deionized water rinsings, can obtain the nano zinc oxide material that nanometer rod aligns through drying naturally after repeatedly washing.
2. synthetic (sulfuration of zinc oxide) of zinc sulfide nano pipe:
A) preparation of vulcanization reaction solution: 1.5 gram thioacetamides according to being dissolved in 100 ml deionized water, are stirred to the solution clarification, can be prepared into vulcanization reaction solution.
B) synthetic (sulfuration of zinc oxide) of the zinc sulfide nano-material that aligns of nanotube: from the above-mentioned vulcanization reaction solution for preparing, take out 30 milliliters, pour in 40 milliliters the tetrafluoroethylene inner bag, the zinc oxide nano film for preparing in advance vertically is immersed in the vulcanization reaction solution, airtight water heater container, pack in the stainless steel cauldron, be warming up to 130 ℃, reacted 47 hours, reaction naturally cools to normal temperature after finishing, take out the sample deionized water rinsing, can obtain the zinc sulfide nano-material that nanotube aligns through drying naturally after repeatedly washing.
Embodiment 3
1. the preparation of the nano zinc oxide material that aligns of nanometer rod:
A) preparation of chemically grown reaction solution: zinc nitrate hexahydrate, thiocarbamide, ammoniacal liquor and ammonium chloride are dissolved in deionized water by a certain percentage, be prepared into the film growth reaction solution, contain zinc nitrate hexahydrate 0.01mol, 25% (mass ratio) ammoniacal liquor 5ml, thiocarbamide 0.01mol and ammonium chloride 0002mol in every 100ml aqueous solution;
B) pre-treatment of substrate: at first quartz substrate was immersed in the vitriol oil of ebullient 98% 10 hours, was immersed in then in the acetone ultrasonic 60 minutes, next use a large amount of deionized water rinsings, at last substrate is dried in vacuum drying oven, stand-by.
C) nano zinc oxide material that aligns of nanometer rod is synthetic: before reaction, at first substrate is soaked in the above-mentioned chemically grown reaction soln for preparing; Reaction system is warming up to 95 ℃ again, temperature rise rate 15 degree/minute, reacted 60 minutes down at 95 ℃.Reaction finishes the back cools off fast with frozen water, substrate is put in deionized water for ultrasonic 1 minute then, uses a large amount of deionized water rinsings, can obtain the nano zinc oxide material that nanometer rod aligns through drying naturally after repeatedly washing.
2. synthetic (sulfuration of zinc oxide) of the zinc sulfide nano-material that aligns of nanotube:
A) preparation of vulcanization reaction solution: 3 gram thioacetamides according to being dissolved in 200 ml deionized water, are stirred to the solution clarification, can be prepared into vulcanization reaction solution.
B) synthetic (sulfuration of zinc oxide) of the zinc sulfide nano-material that aligns of nanotube: from the above-mentioned vulcanization reaction solution for preparing, take out 30 milliliters, pour in 40 milliliters the tetrafluoroethylene inner bag, the zinc oxide nano film for preparing in advance vertically is immersed in the vulcanization reaction solution, airtight water heater container, pack in the stainless steel cauldron, be warming up to 130 ℃, reacted 48 hours, reaction naturally cools to normal temperature after finishing, take out the sample deionized water rinsing, can obtain the zinc sulfide nano-material that nanotube aligns through drying naturally after repeatedly washing.
Claims (2)
1, the preparation method of the zinc sulfide nano-material that aligns of a kind of nanotube is characterized in that comprising the steps:
1) preparation of the nano zinc oxide material that aligns of nanometer rod: zinc salt, thiocarbamide, ammoniacal liquor and ammonium salt are dissolved in deionized water in proportion, be prepared into the film growth reaction solution, contain zinc salt 0.01mol, mass ratio in every 100ml reaction solution and be 25% ammoniacal liquor 5ml, thiocarbamide 0.01mol and ammonium salt 0.002mol; The substrate that is selected from sheet glass or quartz plate was immersed in the vitriol oil of ebullient 98% 5～10 hours, be immersed in then in the acetone ultrasonic 30～60 minutes, with drying behind the deionized water rinsing, substrate is soaked in the above-mentioned reaction solution, reaction system is warming up to 94～97 ℃, temperature rise rate 10～20 degree/minute, reacted 45～60 minutes down at 94～97 ℃, reaction finishes back cooling fast, substrate was put in deionized water for ultrasonic 1～2 minute then, with drying naturally behind the deionized water wash, obtain the nano zinc oxide material that nanometer rod aligns;
2) zinc sulfide nano-material that aligns of nanotube is synthetic: sulphur source thioacetamide is dissolved in the deionized water, be stirred to the solution clarification, being prepared into sulphur source concentration is the vulcanization reaction solution of 1.5 grams/100 ml waters, the nano zinc oxide material for preparing vertically is immersed in the above-mentioned vulcanization reaction solution, closed reaction vessel, pack in the stainless steel cauldron, be warming up to 130 ℃, reacted 47-49 hour, reaction naturally cools to normal temperature after finishing, take out sample and dry naturally after with deionized water wash, can obtain the zinc sulfide nano-material that nanotube aligns.
2, the preparation method of the zinc sulfide nano-material that aligns of nanotube as claimed in claim 1 is characterized in that described zinc salt is a zinc nitrate hexahydrate, and ammonium salt is an ammonium chloride.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| AU2006233503A1 (en) * | 2005-04-14 | 2006-10-19 | Tallinn University Of Technology | Method of preparing zinc oxide nanorods on a substrate by chemical spray pyrolysis |
| CN100335414C (en) * | 2005-09-02 | 2007-09-05 | 清华大学 | Zinc sulfide microsphere synthesis method |
| CN100436661C (en) * | 2006-01-27 | 2008-11-26 | 北京大学 | Method for in situ growth for preparing semiconductor nanotube |
| CN101127308B (en) * | 2007-09-14 | 2011-10-05 | 中国科学院上海硅酸盐研究所 | A method for sinking non crystal ZnS film under room temperature condition |
| CN102897849A (en) * | 2012-10-10 | 2013-01-30 | 华中科技大学 | Method of preparing super-capacitor electrode material |
| CN107673401A (en) * | 2017-10-25 | 2018-02-09 | 广西沙田仙人滩农业投资有限公司 | A kind of preparation method of nanoscale ZnS films |
| CN114436639A (en) * | 2020-11-04 | 2022-05-06 | 天津理工大学 | ZnO-based thermoelectric ceramic with high thermoelectric performance and preparation method thereof |
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