CN102961983A - Method for dissolving selenium in ethanol - Google Patents
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- CN102961983A CN102961983A CN2012104223989A CN201210422398A CN102961983A CN 102961983 A CN102961983 A CN 102961983A CN 2012104223989 A CN2012104223989 A CN 2012104223989A CN 201210422398 A CN201210422398 A CN 201210422398A CN 102961983 A CN102961983 A CN 102961983A
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Abstract
The invention discloses a method for dissolving selenium in ethanol and belongs to the technical field of nano-material. The method comprises dissolution of selenium in ethanol and proving of dissolution. According to the method, a selenium powder is acted by laser method in ethanol to obtain a colorless transparent liquid, and metal target material is acted in the solution to obtain a nuclear shell structure, so as to illustrate solubility of selenium in ethanol. The invention provides a simply operated and green method for dissolving selenium; and the method does not require complex equipment, and is simple and efficient. The method for dissolving selenium in ethanol provided by the invention provides a green non-toxic selenium source for further synthesis of selenide nano crystalline.
Description
Technical field
The invention belongs to technical field of nano material, more particularly, particularly a kind of method that selenium powder is dissolved in ethanol.
Background technology
Semiconductor nano since significant quantum size less than, therefore their photophysical property and chemical property become rapidly one of present most active research field, and wherein the characteristics such as the supper-fast optical nonlinearity response that has of Nano semiconductor particles and luminescence generated by light get most of the attention.Because having excellent light transfer characteristic, the porous Large ratio surface PEC battery that semi-conductor nano particles consists of impel numerous scientists that the nanocrystal photovoltaic cell has been carried out large quantity research simultaneously.Wherein selenide semiconductor nanocrystalline because of its unique physical chemical property that is different from body phase material because of it widely research, they have a wide range of applications in various fields, comprise solar cell, biomarker and diagnosis, nano photoelectric device etc.Silver selenide such as non-stoichiometric has huge magnetic.Therefore, the nanocrystalline synthetic technology of development selenide semiconductor and to explore its excellent performance significant for modern science and technology.
Generally speaking, preparing the nanocrystalline method of selenides, to generally comprise vapor phase method and liquid phase synthetic.Because the equipment that vapor phase method needs is complexity and product yield is few, productive rate is low.Since Bawendi in 1993 etc. in organic solvent since synthetic single method of disperseing semiconductor-quantum-point, the synthetic selenides of liquid phase method is nanocrystalline has obtained fast development.However, these liquid phase building-up processes are usually owing to the selection of selenium source is restricted, selenium powder is dissolved in the concentrated sulfuric acid, chloroform, be slightly soluble in carbon disulfide, water insoluble, ethanol, so generally can select hypertoxic tri octyl phosphine TOP to dissolve selenium powder as solvent, so that the process of preparation selenides can't realize nontoxic, green, environmental protection fully, so the dissolution problems that solves selenium powder prepares for green, and selenides is nanocrystalline a very important effect.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of selenium powder that improves in the deliquescent method of ethanol, the method preparation process is simple, production operation safety, and production cost is low.
In order to solve the problems of the technologies described above, the present invention is achieved by following technical scheme:
A kind of method that selenium is dissolved in ethanol, selenium powder is placed ethanol, pass into inert gas to remove the interference of oxygen, then utilize laser action selenium powder-ethanol system, to obtain pink solution, carry out at last the centrifugal water white transparency supernatant that can obtain being dissolved with selenium.
Utilize the HTHP of laser to impel selenium powder that certain dissolubility is arranged in ethanol, selenium powder will be still in the solution bottom during laser action.To pass into first inert gas (for example argon gas) during laser action and remove residual oxygen in the container.After obtaining to be dissolved with the water white transparency supernatant of selenium, its selenium source as green further can be used, for example the effect metal targets obtains nucleocapsid structure in this solution.Select the Nd:YAG millisecond pulse laser of Wuhan Chinese workers' laser engineering Co., Ltd, the power that effect selenium powder-ethanol system is selected is 50W-400W, and pulse width is 1ms-10ms, and repetition rate is 10HZ-20HZ, and be 1-5min action time; The power that effect cadmium target is selected is 200W-400W, and pulse width is 6ms-10ms, and repetition rate is 1-5HZ, and be 5-15min action time.
The present invention acts on selenium powder with laser method in ethanol, obtain water white transparency shape liquid, the effect metal targets obtains nucleocapsid structure in this solution again, the dissolubility of selenium in ethanol has been described, shown in accompanying drawing 1-4, after the selenium powder solution ethanol laser action change color as shown in Figure 1, as can be seen from the figure original clear solution becomes red solution, Figure 2 shows that the ESEM pattern picture of above-mentioned red solution, Figure 3 shows that the XRD result of above-mentioned red solution.Figure 4 shows that the nucleocapsid structure that effect cadmium target obtains in the clear solution after above-mentioned red solution is centrifugal, can verify has the existence of selenium this moment in the ethanol.The invention provides a kind of method of easy and simple to handle, green dissolved selenium, do not need complex apparatus.The method is simple, efficient, and the method that selenium is dissolved in the ethanol provided by the invention provides a kind of green non-poisonous selenium source for nanocrystalline synthetic of later selenides.
Description of drawings
Fig. 1 is the photo of the red selenium solution for preparing of the present invention, and the left side is the photo before the laser action, and the right side is the photo after the laser action
Fig. 2 is the ESEM pattern picture (Electronic Speculum is the S-4800 field emission scanning electron microscope of HITACHI company) of the red selenium solution for preparing of the present invention
Fig. 3 is XRD result's (instrument is Rigaku Rigaku D/MAX 2500 type X ray polycrystal powder diffractometers) of the red selenium solution for preparing of the present invention
Fig. 4 is the transmission electron microscope pattern picture (Electronic Speculum is the Tecnai G2F20 field transmission electron microscope of FEI Co.) of the cadmium selenide bag cadmium for preparing of the present invention
The specific embodiment
Further specify technical scheme of the present invention below in conjunction with specific embodiment.Select the Nd:YAG millisecond pulse laser of Wuhan Chinese workers' laser engineering Co., Ltd.
Embodiment 1
[1] weighing 0.02g selenium powder is dissolved in the ethanol, passes into the interference that argon gas is removed oxygen
[2] above-mentioned 1064 milliseconds of laser instruments are adopted in experiment, and the presoma of action step ⑴ preparation obtains pink solution, and power is 400W, and pulse width is 1ms, and repetition rate is 10HZ, and be 1min action time
[3] red solution with step [2] obtains the water white transparency supernatant with the centrifugal 30min of 10000r.
[4] choose certain laser parameter effect Cd target in the supernatant that step [3] obtains, power is 200W, and pulse width is 10ms, and repetition rate is 5HZ, and be 15min action time
Embodiment 2
⑴ weighing 0.02g selenium powder is dissolved in the ethanolic solution, passes into the interference that argon gas is removed oxygen
[2] above-mentioned 1064 milliseconds of laser instruments are adopted in experiment, and the presoma of action step ⑴ preparation obtains pink solution, and power is 50W, and pulse width is 10ms, and repetition rate is 20HZ, and be 5min action time
[3] red solution with step [2] obtains the water white transparency supernatant with the centrifugal 30min of 10000r.
[4] choose certain laser parameter effect Cd target in the supernatant that step [3] obtains, power is 400W, and pulse width is 6ms, and repetition rate is 1HZ, and be 5min action time
Embodiment 3
⑴ weighing 0.02g selenium powder is dissolved in the ethanolic solution of 20ml, passes into the interference that argon gas is removed oxygen
[2] above-mentioned 1064 milliseconds of laser instruments are adopted in experiment, and the presoma of action step ⑴ preparation obtains pink solution, and power is 200W, and pulse width is 5ms, and repetition rate is 15HZ, and be 3min action time
[3] red solution with step [2] obtains the water white transparency supernatant with the centrifugal 30min of 10000r.
[4] choose certain laser parameter effect Cd target in the supernatant that step [3] obtains, power is 300W, and pulse width is 8ms, and repetition rate is 3HZ, and be 10min action time
Embodiment 4
[1] weighing 0.02g selenium powder is dissolved in the ethanolic solution of 20ml, passes into the interference that argon gas is removed oxygen
[2] above-mentioned 1064 milliseconds of laser instruments are adopted in experiment, and the presoma of action step ⑴ preparation obtains pink solution, and power is 100W, and pulse width is 8ms, and repetition rate is 12HZ, and be 4min action time
[3] red solution with step [2] obtains the water white transparency supernatant with the centrifugal 30min of 10000r.
[4] choose certain laser parameter effect Cd target in the supernatant that step [3] obtains, power is 350W, and pulse width is 7ms, and repetition rate is 2HZ, and be 8min action time
Embodiment 5
[1] a certain amount of selenium powder of weighing is dissolved in the ethanol, passes into the interference that argon gas is removed oxygen
[2] above-mentioned 1064 milliseconds of laser instruments are adopted in experiment, and the presoma of action step ⑴ preparation obtains pink solution, and power is 300W, and pulse width is 3ms, and repetition rate is 18HZ, and be 2min action time
[3] red solution with step [2] obtains the water white transparency supernatant with the centrifugal 30min of 10000r.
[4] effect Cd target in the supernatant that step [3] obtains, power is 250W, pulse width is 8ms, repetition rate is 4HZ, action time 12min
More than the present invention has been done exemplary description; should be noted that; in the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (3)
1. one kind is dissolved in the method for ethanol with selenium, it is characterized in that, selenium powder is placed ethanol, pass into inert gas to remove the interference of oxygen, then utilize laser action selenium powder-ethanol system, to obtain pink solution, carry out at last the centrifugal water white transparency supernatant that can obtain being dissolved with selenium.
2. a kind of method that selenium is dissolved in ethanol according to claim 1, it is characterized in that, selenium powder will be still in the solution bottom during laser action, select the Nd:YAG millisecond pulse laser of Wuhan Chinese workers' laser engineering Co., Ltd, the power that effect selenium powder-ethanol system is selected is 50W-400W, pulse width is 1ms-10ms, and repetition rate is 10HZ-20HZ, and be 1-5min action time.
3. utilize a kind of method that selenium is dissolved in ethanol as claimed in claim 1 to prepare the method for metal core shell structure, it is characterized in that, after obtaining to be dissolved with the water white transparency supernatant of selenium, with its selenium source as green, the effect metal targets obtains nucleocapsid structure in this solution, select the Nd:YAG millisecond pulse laser of Wuhan Chinese workers' laser engineering Co., Ltd, the power that effect cadmium target is selected is 200W-400W, pulse width is 6ms-10ms, repetition rate is 1-5HZ, and be 5-15min action time.
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| CN201210422398.9A CN102961983B (en) | 2012-10-29 | 2012-10-29 | Method for dissolving selenium in ethanol |
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| CN201210422398.9A CN102961983B (en) | 2012-10-29 | 2012-10-29 | Method for dissolving selenium in ethanol |
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| CN102961983B CN102961983B (en) | 2014-05-21 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108728651A (en) * | 2018-06-01 | 2018-11-02 | 汉能新材料科技有限公司 | A kind of recovery method of selenium |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401451A (en) * | 2002-09-21 | 2003-03-12 | 福建师范大学 | Method for continuous preparation of nano-metal, alloy and their mixture sol |
| CN101186825A (en) * | 2007-11-15 | 2008-05-28 | 合肥工业大学 | Selenium precursor fluid and method for preparing cadmium selenide or zinc selenide quantum dots by using the same |
| CN102717083A (en) * | 2012-05-28 | 2012-10-10 | 天津大学 | Method for preparing cadmium metal nano particles by laser |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401451A (en) * | 2002-09-21 | 2003-03-12 | 福建师范大学 | Method for continuous preparation of nano-metal, alloy and their mixture sol |
| CN101186825A (en) * | 2007-11-15 | 2008-05-28 | 合肥工业大学 | Selenium precursor fluid and method for preparing cadmium selenide or zinc selenide quantum dots by using the same |
| CN102717083A (en) * | 2012-05-28 | 2012-10-10 | 天津大学 | Method for preparing cadmium metal nano particles by laser |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108728651A (en) * | 2018-06-01 | 2018-11-02 | 汉能新材料科技有限公司 | A kind of recovery method of selenium |
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