CN105036092A - Preparation method of spherical silver selenide particles - Google Patents
Preparation method of spherical silver selenide particles Download PDFInfo
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- CN105036092A CN105036092A CN201510479135.5A CN201510479135A CN105036092A CN 105036092 A CN105036092 A CN 105036092A CN 201510479135 A CN201510479135 A CN 201510479135A CN 105036092 A CN105036092 A CN 105036092A
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Abstract
The invention discloses a preparation method of spherical silver selenide particles. The method comprises the steps that selenium powder and a silver-ammonia complex serve as raw materials to react in organic solvent at the temperature ranging from 160 DEG C to 220 DEG C for 4-24 h, and the spherical silver selenide particles are prepared after cleaning and drying are conducted. According to the preparation method of the spherical silver selenide particles, the selenium powder and the silver-ammonia complex serve as the raw materials, ethylene glycol serves as the solvent and a reducing agent, and the toxicity and the pollution to the environment are small in the preparation process; the prepared Ag2Se is good in dispersity, the particle size ranges fromm 50 nm to 500 nm, and the preparation method of the spherical silver selenide particles can be used for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of silver selenide, particularly relate to a kind of preparation method of spherical silver selenide particle.
Background technology
Ag
2se belongs to non magnetic low-gap semiconductor, is one of semiconductor material with great using value.Ag
2se has two kinds of stable phase structures: low temperature bata phase and high temperature α phase.Silver selenide transformation temperature is 133 DEG C, low-temperature phase β-Ag
2se belongs to the semiconductor material of narrow band gap, has relatively high Seebeck coefficient, lower thermal conductivity and high conductivity, is widely used in optical material and thermoelectric material field as photosensitizers; Recent study finds another low temperature metastable phase t-Ag at nano thin-film and nanocrystalline middle existence
2se, has potential using value in photoelectricity, thermoelectricity field equally.High-temperature-phase α-Ag
2se material is a kind of superionic conductor(s), can be applicable to the fields such as device for non-linear optical, solar cell and multifunction ion choice electrode.In addition, the silver selenide Ag of non-metering chemical ratio
2+ δse has linear positive magnetoresistance, and its characteristic has great using value in magnetic recording and high-intensity magnetic field detection.
At present, Ag is prepared
2the method of Se micro Nano material mainly contains hydrothermal method, solvent-thermal method, template, electrochemical process, microemulsion method, chemical deposition method etc." preparation method of silver selenide nanometer material " disclosed in Chinese patent literature CN101555000A employs nitrogen atmosphere protection, adds technology difficulty; " a kind of synthetic method of silver selenide nanospheres " disclosed in patent documentation CN101575088A is not easy to obtain for raw material, raw material with Silver Nitrate, selenophen, aniline, desired reaction temperature 240 DEG C, and silver selenide nanospheres is reunited serious; " a kind of method preparing monodisperse nanometer semiconductor selenide particle " disclosed in patent documentation CN1772599A needs to add alkali metal hydroxide and lipid acid, and is reductive agent with hydrazine hydrate, and toxicity is comparatively large, high to operational requirement; " preparation method of single dispersing silver, silver sulfide and selenide nanocrystal " disclosed in patent documentation CN101274751A first high temperature thermal decomposition Silver Nitrate, then add selenium powder reaction, be mainly the silver selenide nanoparticle of 6 ~ 12nm, and need two step operations.Visible, existing preparation Ag
2the technology of Se micro Nano material often needs inert atmosphere protection or needs to configure the precursor solution complicated, toxicity is larger; or equipment is complicated, with high costs; and be difficult to large-scale production, also there is reunion in the nanoparticle obtained, is therefore difficult to realize its industrial applications.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, there is provided that a kind of technique is simple, environmental pollution is little, toxicity is little, the preparation method of the spherical silver selenide particle that product dispersing property is good, the silver selenide of preparation has very large using value in photoelectricity, thermoelectricity field.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is:
A preparation method for spherical silver selenide particle, with selenium powder and silver-colored amine complex for raw material, in organic solvent, reacts cleaning, drying after 4 ~ 24 hours and makes spherical silver selenide particle at 160 ~ 220 DEG C of temperature.
Above-mentioned preparation method, preferably, its preparation method specifically comprises the following steps:
1) add in organic solvent by Silver Nitrate, selenium powder, strong aqua, dispersion agent, ultrasonic disperse is even, obtains reaction solution;
2) by step 1) in the reaction solution of preparation to be placed at 160 ~ 220 DEG C of temperature reaction 4 ~ 24 hours, naturally cool to room temperature, centrifugally obtain silver selenide precipitated product;
3) by step 2) the silver selenide precipitated product washes of absolute alcohol that obtains 2 ~ 5 times, then at the silver selenide after cleaning is placed in 50 ~ 70 DEG C dry 6 ~ 8 hours, namely obtain described spherical silver selenide particle.
Above-mentioned preparation method, preferably, described step 1) in, dispersion agent is polyvinylpyrrolidone.
Above-mentioned preparation method, preferably, described step 1) in, organic solvent is one or more in ethanol, ethylene glycol, glycerol.
Above-mentioned preparation method, preferably, described step 1) in, the time of ultrasonic disperse is 5 ~ 10min.
Above-mentioned preparation method, preferably, described step 1) in, in Silver Nitrate, the mol ratio of silver atoms and selenium powder selenium atom is 2:1, the quality of dispersion agent is 0.5 ~ 5 times of Silver Nitrate quality, and strong aqua add-on is make Silver Nitrate form 1 ~ 3 times of the theoretical amount of silver-colored amine complex.
Principle of the present invention: take ethylene glycol as solvent and reductive agent, silver-colored amine complex is reduced to silver-colored simple substance, then generates silver selenide with selenium reaction.Ethylene glycol, as reductive agent, will be first aldehyde through high temperature slow oxidation, the more silver-colored ammonia of slow reduction; With silver-colored ammonia for title complex object slows down reduction rate, thus obtain good dispersity, the silver selenide particle of uniform particle diameter.
Compared with prior art, the invention has the advantages that:
1) preparation method of the present invention is with selenium powder and silver-colored amine complex for raw material, and adopt closed reactor heating, preparation process toxic is little, environmental pollution is little.
2) the present invention is using ethylene glycol as solvent and reductive agent, and sluggish is carried out, and can prepare good dispersity, particle diameter is the Ag of 50 ~ 500nm
2se, can be used for suitability for industrialized production.
3) preparation method of the present invention adopts disposable reinforced, and do not need to prepare complicated precursor solution, technological operation is simple, and equipment requirements is low, is easy to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of spherical silver selenide particle prepared by the embodiment of the present invention 1.
Fig. 2 is spherical silver selenide nano particle EDS ultimate analysis collection of illustrative plates prepared by the embodiment of the present invention 1.
Embodiment
For the ease of understanding the present invention, hereafter will do to describe more comprehensively, meticulously to the present invention in conjunction with Figure of description and preferred embodiment, but protection scope of the present invention is not limited to following specific embodiment.
Unless otherwise defined, hereinafter used all technical terms are identical with the implication that those skilled in the art understand usually.The object of technical term used herein just in order to describe specific embodiment is not be intended to limit the scope of the invention.
Apart from special instruction, all ingredients used in the present invention, raw material are can commodity commercially or can by the obtained product of known method.
Embodiment 1:
A preparation method for spherical silver selenide particle of the present invention, comprises the following steps:
1) taking 0.34g Silver Nitrate, 0.08g selenium powder, 0.5g polyvinylpyrrolidone, 2mL strong aqua and 33mL ethylene glycol joins in stainless steel cauldron, and ultrasonic disperse obtains reaction solution to being uniformly dispersed in 5 minutes.
2) by step 1) reaction solution that obtains is heated to 200 DEG C, and react after 12 hours, naturally cool to room temperature, more centrifugal (centrifugal settling rotating speed is 10000 revs/min) obtains silver selenide precipitated product.
3) by step 2) the silver selenide precipitated product absolute ethanol washing that obtains three times, then the silver selenide precipitated product after cleaning is placed in vacuum drying oven, at 50 DEG C dry 8 hours, obtains spherical silver selenide particle.
As shown in Figure 1, as can be seen from Figure 1 silver selenide particle is spherical in shape, and median size is 300nm for spherical silver selenide particle stereoscan photograph prepared by the present embodiment.
Spherical silver selenide nano particle EDS ultimate analysis collection of illustrative plates prepared by the present embodiment as shown in Figure 2, analyze EDS result from Fig. 2 and only have Ag, Se, Cu, O tetra-kinds of elements, Cu derives from copper mesh when EDS detects, and micro-O is the O in silver selenide surface organic matter PVP.
Embodiment 2:
A preparation method for spherical silver selenide particle of the present invention, comprises the following steps:
1) taking 0.34g Silver Nitrate, 0.08g selenium powder, 1.0g polyvinylpyrrolidone, 1mL strong aqua and 34mL ethylene glycol joins in stainless steel cauldron, and ultrasonic disperse obtains reaction solution to being uniformly dispersed in 5 minutes.
2) by step 1) reaction solution that obtains is heated to 180 DEG C, and react after 10 hours, naturally cool to room temperature, more centrifugal (centrifugal settling rotating speed is 10000 revs/min) obtains silver selenide precipitated product.
3) by step 2) the silver selenide precipitated product absolute ethanol washing that obtains five times, then the silver selenide precipitated product after cleaning is placed in vacuum drying oven, at 50 DEG C dry 8 hours, obtains spherical silver selenide particle.
Carry out electron-microscope scanning to spherical silver selenide particle prepared by the present embodiment, find out that silver selenide particle is spherical in shape from electron-microscope scanning figure, median size is 120nm.
Embodiment 3:
A preparation method for spherical silver selenide particle of the present invention, comprises the following steps:
1) taking 0.34g Silver Nitrate, 0.08g selenium powder, 0.5g polyvinylpyrrolidone, 0.6mL strong aqua and 34.4mL ethylene glycol joins in stainless steel cauldron, and ultrasonic disperse 5 clock, to being uniformly dispersed, obtains reaction solution.
2) by step 1) reaction solution that obtains is heated to 180 DEG C, and react after 4 hours, naturally cool to room temperature, more centrifugal (centrifugal settling rotating speed is 10000 revs/min) obtains silver selenide precipitated product.
3) by step 2) the silver selenide absolute ethanol washing that obtains three times, then the silver selenide precipitated product after cleaning is placed in vacuum drying oven, at 60 DEG C dry 8 hours, obtains spherical silver selenide particle.
Carry out electron-microscope scanning to spherical silver selenide particle prepared by the present embodiment, from electron-microscope scanning figure, find out that silver selenide particle is that class is spherical, median size is 150nm.
Claims (6)
1. a preparation method for spherical silver selenide particle, is characterized in that, with selenium powder and silver-colored amine complex for raw material, in organic solvent, reacts cleaning, drying after 4 ~ 24 hours make spherical silver selenide particle at 160 ~ 220 DEG C of temperature.
2. preparation method as claimed in claim 1, it is characterized in that, its preparation method specifically comprises the following steps:
1) add in organic solvent by Silver Nitrate, selenium powder, strong aqua, dispersion agent, ultrasonic disperse is even, obtains reaction solution;
2) by step 1) reaction solution prepared to be placed at 160 ~ 220 DEG C of temperature reaction 4 ~ 24 hours, naturally cools to room temperature, centrifugally obtains silver selenide precipitated product;
3) by step 2) the silver selenide precipitated product washes of absolute alcohol that obtains 2 ~ 5 times, then at the silver selenide after cleaning is placed in 50 ~ 70 DEG C dry 6 ~ 8 hours, namely obtain described spherical silver selenide particle.
3. preparation method as claimed in claim 2, is characterized in that, described step 1) in, dispersion agent is polyvinylpyrrolidone.
4. preparation method as claimed in claim 2, is characterized in that, described step 1) in, organic solvent be ethanol, ethylene glycol, glycerol one or more.
5. preparation method as claimed in claim 2, is characterized in that, described step 1) in, the time of ultrasonic disperse is 5 ~ 10min.
6. the preparation method as described in any one of claim 2 ~ 5, it is characterized in that, described step 1) in, in Silver Nitrate, in silver atoms and selenium powder, the mol ratio of selenium atom is 2:1, the quality of dispersion agent is 0.5 ~ 5 times of Silver Nitrate quality, and the add-on of strong aqua is make Silver Nitrate form 1 ~ 3 times of the theoretical amount of silver-colored amine complex.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106978182B (en) * | 2017-03-17 | 2019-04-19 | 中南大学 | A kind of preparation method for the water-soluble selenizing silver content point quickly preparing size tunable |
| CN109806891A (en) * | 2019-03-25 | 2019-05-28 | 东华大学 | A kind of Ag2The preparation method and application of Se/GO micro-flowers structure nano material |
| CN111774037A (en) * | 2020-07-14 | 2020-10-16 | 湖北大学 | Preparation method of ZIF-67-silver selenide nanocomposite |
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| CN1709618A (en) * | 2005-07-08 | 2005-12-21 | 昆明理工大学 | Method for preparing nano or submicron silver powder |
| CN1772599A (en) * | 2005-10-19 | 2006-05-17 | 清华大学 | Process of preparing monodisperse nanometer semiconductor selenide particle |
| CN101274751A (en) * | 2007-03-30 | 2008-10-01 | 清华大学 | Preparation for monodisperse, argentic sulfide and silver selenide nanocrystal |
| CN102085574A (en) * | 2009-12-04 | 2011-06-08 | 深圳先进技术研究院 | Water-dispersible silver nanometer particles and preparation method thereof |
| CN103286323A (en) * | 2013-05-02 | 2013-09-11 | 中冶陕压重工设备有限公司 | Method for processing long thin-walled sleeve parts by utilizing tyre-expansion type mandrel |
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- 2015-08-07 CN CN201510479135.5A patent/CN105036092B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709618A (en) * | 2005-07-08 | 2005-12-21 | 昆明理工大学 | Method for preparing nano or submicron silver powder |
| CN1772599A (en) * | 2005-10-19 | 2006-05-17 | 清华大学 | Process of preparing monodisperse nanometer semiconductor selenide particle |
| CN101274751A (en) * | 2007-03-30 | 2008-10-01 | 清华大学 | Preparation for monodisperse, argentic sulfide and silver selenide nanocrystal |
| CN102085574A (en) * | 2009-12-04 | 2011-06-08 | 深圳先进技术研究院 | Water-dispersible silver nanometer particles and preparation method thereof |
| CN103286323A (en) * | 2013-05-02 | 2013-09-11 | 中冶陕压重工设备有限公司 | Method for processing long thin-walled sleeve parts by utilizing tyre-expansion type mandrel |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106978182B (en) * | 2017-03-17 | 2019-04-19 | 中南大学 | A kind of preparation method for the water-soluble selenizing silver content point quickly preparing size tunable |
| CN109806891A (en) * | 2019-03-25 | 2019-05-28 | 东华大学 | A kind of Ag2The preparation method and application of Se/GO micro-flowers structure nano material |
| CN111774037A (en) * | 2020-07-14 | 2020-10-16 | 湖北大学 | Preparation method of ZIF-67-silver selenide nanocomposite |
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