CN107099811A - The preparation method of selenium nanowires - Google Patents
The preparation method of selenium nanowires Download PDFInfo
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- CN107099811A CN107099811A CN201710368088.6A CN201710368088A CN107099811A CN 107099811 A CN107099811 A CN 107099811A CN 201710368088 A CN201710368088 A CN 201710368088A CN 107099811 A CN107099811 A CN 107099811A
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- Prior art keywords
- selenium
- preparation
- hydrochloric acid
- polyethylene glycol
- sodium selenite
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention provides a kind of preparation method of selenium nanowires, including：a）It is electrolysed using sodium selenite, polyethylene glycol and aqueous hydrochloric acid solution as electrolyte, obtains selenium simple substance；b）Aging is stood after the selenium simple substance is washed in absolute ethyl alcohol, selenium nanowires are obtained.The present invention is electrolysed using sodium selenite, polyethylene glycol and aqueous hydrochloric acid solution as electrolyte, and sodium selenite is reduced to elemental selenium in negative electrode, and hydrochloric acid provides the progress that sour environment is beneficial to reduction reaction；Polyethylene glycol plays peptizaiton so that precipitation particle is tiny, beneficial to the transformation of follow-up crystal formation, shortens the time of generation selenium nanowires.Obtain after elemental selenium, it is stood to aging in absolute ethyl alcohol, elemental selenium can convert to form nano wire.Test result indicates that, the method that the present invention is provided obtains selenium nanowires.
Description
Technical field
The invention belongs to nanowire technique field, more particularly to a kind of preparation method of selenium nanowires.
Background technology
Se is a kind of important element semiconductor, with many excellent photoelectric properties.In the last few years, as people are to list
Matter nanostructured research is goed deep into, and the quantum confined effect of selenium and unique anisotropy feature are gradually attracted much attention,
The construction unit of nano photoelectronic devices as a new generation, is building electricity, photoelectric device, the nonlinear optics of nanoscale
There is good application prospect in terms of material and catalysis material.
So far, prior art has proposed the method for many chemical synthesis in liquid phase selenium nanowires, such as heating reflux method, molten
Agent（Water）Hot method, sonochemical method, Microwave-assisted synthesis method, photo-thermal auxiliary synthetic method, biomolecule template etc..Although these
Synthetic method controls the growth of Se one-dimensional nano structures well, but most methods are still more complicated, it is necessary to template, outer
Plus the auxiliary and the reaction condition of harshness of crystal seed, bring difficulty to large-scale synthesis.Therefore green, efficient conjunction are developed
New method into Se one-dimensional nano structures has great importance.
The content of the invention
In view of this, it is an object of the invention to provide a kind of preparation method of selenium nanowires, apparatus and method are more simple
Single, reaction condition is gentle.
The invention provides a kind of preparation method of selenium nanowires, including：
a）It is electrolysed using sodium selenite, polyethylene glycol and aqueous hydrochloric acid solution as electrolyte, obtains selenium simple substance；
b）Aging is stood after the selenium simple substance is washed in absolute ethyl alcohol, selenium nanowires are obtained.
The present invention is electrolysed using sodium selenite, polyethylene glycol and aqueous hydrochloric acid solution as electrolyte, and sodium selenite is in the moon
Pole is reduced to elemental selenium, and hydrochloric acid provides the progress that sour environment is beneficial to reduction reaction；Polyethylene glycol plays peptizaiton so that heavy
Shallow lake particle is tiny, beneficial to the transformation of follow-up crystal formation, shortens the time of generation selenium nanowires.Obtain after elemental selenium, by it anhydrous
Aging is stood in ethanol, elemental selenium can convert to form nano wire.Test result indicates that, the method that the present invention is provided obtains selenium
Nano wire.
The present invention first mixes sodium selenite, polyethylene glycol and hydrochloric acid in water, regard obtained solution as electrolyte.
Wherein, the hydrochloric acid is concentrated hydrochloric acid；The number-average molecular weight of the polyethylene glycol is 200 ~ 800.In the present invention, polyethylene glycol is made
For the addition of dispersant, critical effect is played in the growth to follow-up nano wire, test result indicates that, if be added without scattered
Agent, elemental selenium aging generation nano wire in absolute ethyl alcohol then needs the time of one week.
In the 100mL electrolyte, comprising：
0.5 ~ 2.0g sodium selenite；
2.0 ~ 4.0mL polyethylene glycol；
1 ~ 2mL hydrochloric acid；
With the water of surplus.
In one embodiment, in 100mL electrolyte, comprising：
1g sodium selenite；
3mL polyethylene glycol；
1.5mL hydrochloric acid；
With the water of surplus.
In one embodiment of the invention, it can be electrolysed, be comprised the following steps that in diaphragmless cell：
Using sodium selenite, polyethylene glycol and aqueous hydrochloric acid solution as electrolyte, insertion negative electrode and anode formation diaphragmless cell
It is electrolysed afterwards.
In one embodiment of the invention, it can also be electrolysed, be comprised the following steps that in diaphragm cell：
Using sodium selenite, polyethylene glycol and aqueous hydrochloric acid solution as electrolyte, insertion negative electrode and anode, and will with cation membrane
Negative electrode and anode are separated, and are electrolysed after forming diaphragm cell.
Wherein, the negative electrode is selected from metal electrode film or graphite electrode piece；The anode is selected from graphite electrode piece；The sun
Ion diaphragm is selected from nafion films.Wherein, metal electrode film can be selected from nickel sheet or copper sheet.
In one embodiment of the invention, the temperature of the electrolysis is room temperature, the current density of the electrolysis for 2 ~
15mA/cm2, the electrolysis is constant-current electrolysis.Wherein, the current density of the electrolysis is 3mA/cm2。
After electrolysis is finished, sodium selenite is reduced in hydrochloric environment on negative electrode, forms unformed selenium simple substance precipitation；Will
The washing of precipitate stands in absolute ethyl alcohol and can obtain selenium nanowires after aging.
In one embodiment, distilled water and absolute ethyl alcohol is respectively adopted to wash the selenium simple substance.
In one embodiment, the temperature that aging is stood in absolute ethyl alcohol is room temperature, and the time is 20 ~ 30h.
The present invention is electrolysed using sodium selenite, polyethylene glycol and aqueous hydrochloric acid solution as electrolyte, and sodium selenite is in the moon
Pole is reduced to elemental selenium, and hydrochloric acid provides the progress that sour environment is beneficial to reduction reaction；Polyethylene glycol plays peptizaiton so that heavy
Shallow lake particle is tiny, beneficial to the transformation of follow-up crystal formation, shortens the time of generation selenium nanowires.Obtain after elemental selenium, by it anhydrous
Aging is stood in ethanol, elemental selenium can convert to form nano wire.Test result indicates that, the method that the present invention is provided obtains selenium
Nano wire.
Compared with the existing method for preparing selenium nanowires, the experimental provision and method that the present invention prepares selenium nanowires are simple,
Template need not be used；Without using the poisonous and harmful reagent such as hydrazine hydrate；HTHP is not needed, reaction condition is gentle.
Brief description of the drawings
Fig. 1 is diaphragmless cell structural representation provided in an embodiment of the present invention；
The scanned photograph for the selenium nanowires that Fig. 2 prepares for the method that the present invention is provided；
Fig. 3 is diaphragm cell structure schematic diagram provided in an embodiment of the present invention.
Embodiment
Embodiment 1
（1）By 1.0g sodium selenites, 1.5ml concentrated hydrochloric acids and 3.0ml polyethylene glycol（Mean molecule quantity is 400）It is dissolved in deionized water
The middle formation 100ml aqueous solution；
（2）Negative electrode is made with nickel sheet, graphite cake makees anode and constitutes diaphragmless cell, carried referring to Fig. 1, Fig. 1 for the embodiment of the present invention
The diaphragmless cell structural representation of confession；
（3）At room temperature, with 3mA/cm2The above-mentioned aqueous solution 3.5h of current density constant-current electrolysis, obtain reddish brown precipitation；
（4）Precipitation distilled water, absolute ethyl alcohol are successively washed, then are placed in absolute ethyl alcohol, 24 hours are stood, selenium nanometer is obtained
Line.
Referring to Fig. 2, as a result the scanned photograph for the selenium nanowires that Fig. 2 prepares for the method that the present invention is provided shows, this
The method that invention is provided has prepared selenium nanowires.
Embodiment 2
（1）By 1.0g sodium selenites, 1.5ml concentrated hydrochloric acids and 3.0ml polyethylene glycol（Mean molecule quantity is 400）It is dissolved in deionized water
The middle formation 100ml aqueous solution；
（2）Negative electrode is made with nickel sheet, graphite cake makees anode, separated anode and cathode with nafion films, diaphragm cell is constituted, referring to figure
3, Fig. 3 be diaphragm cell structure schematic diagram provided in an embodiment of the present invention；
（3）At room temperature, with 3mA/cm2The above-mentioned aqueous solution 3.5h of current density constant-current electrolysis, obtain reddish brown precipitation；
（4）Precipitation distilled water, absolute ethyl alcohol are successively washed, then are placed in absolute ethyl alcohol, 24 hours are stood, selenium nanometer is obtained
Line.
As a result show, the method that the present invention is provided has prepared selenium nanowires.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of selenium nanowires, it is characterised in that including：
a）It is electrolysed using sodium selenite, polyethylene glycol and aqueous hydrochloric acid solution as electrolyte, obtains selenium simple substance；
b）Aging is stood after the selenium simple substance is washed in absolute ethyl alcohol, selenium nanowires are obtained.
2. preparation method according to claim 1, it is characterised in that the step a）In, the hydrochloric acid is concentrated hydrochloric acid；
The number-average molecular weight of the polyethylene glycol is 200 ~ 800.
3. preparation method according to claim 2, it is characterised in that the step a）In, in the 100mL electrolyte,
Comprising：
0.5 ~ 2.0g sodium selenite；
2.0 ~ 4.0mL polyethylene glycol；
1 ~ 2mL hydrochloric acid；
With the water of surplus.
4. preparation method according to claim 3, it is characterised in that the step a）In, with sodium selenite, polyethylene glycol
With aqueous hydrochloric acid solution as electrolyte, it is electrolysed after inserting negative electrode and anode formation diaphragmless cell.
5. preparation method according to claim 3, it is characterised in that the step a）In, with sodium selenite, polyethylene glycol
With aqueous hydrochloric acid solution as electrolyte, insertion negative electrode and anode, and negative electrode and anode are separated with cation membrane, form barrier film
It is electrolysed after electrolytic cell.
6. the preparation method according to claim 4 or 5, it is characterised in that the negative electrode is selected from metal electrode film or graphite
Electrode slice；The anode is selected from graphite electrode piece；The cation membrane is selected from nafion films.
7. preparation method according to claim 6, it is characterised in that the temperature of the electrolysis is room temperature, the electrolysis
Current density is 2 ~ 15mA/cm2, the electrolysis is constant-current electrolysis.
8. preparation method according to claim 1, it is characterised in that the step b）, distilled water is respectively adopted and anhydrous
Ethanol is washed to the selenium simple substance.
9. preparation method according to claim 8, it is characterised in that the step b）In, stood in absolute ethyl alcohol old
The temperature of change is room temperature, and the time is 24 ~ 48h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710368088.6A CN107099811A (en) | 2017-05-23 | 2017-05-23 | The preparation method of selenium nanowires |
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| CN201710368088.6A CN107099811A (en) | 2017-05-23 | 2017-05-23 | The preparation method of selenium nanowires |
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| CN107099811A true CN107099811A (en) | 2017-08-29 |
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| CN201710368088.6A Pending CN107099811A (en) | 2017-05-23 | 2017-05-23 | The preparation method of selenium nanowires |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110801438A (en) * | 2019-12-07 | 2020-02-18 | 安徽克菱保健科技有限公司 | Nano-selenium effervescent tablet and preparation method thereof |
| CN112813449A (en) * | 2020-12-31 | 2021-05-18 | 有研国晶辉新材料有限公司 | Method for preparing hydrogen selenide by continuously electrolyzing selenious acid |
| CN112853376A (en) * | 2020-12-31 | 2021-05-28 | 有研国晶辉新材料有限公司 | Method for preparing hydrogen selenide by membrane electrode method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090283411A1 (en) * | 2008-05-15 | 2009-11-19 | Serdar Aksu | Selenium electroplating chemistries and methods |
| CN101759159A (en) * | 2009-12-24 | 2010-06-30 | 暨南大学 | Method for manufacturing nano-selenium in liquid phase and obtained nano-selenium thereof |
| CN105420779A (en) * | 2015-12-03 | 2016-03-23 | 西南石油大学 | Method for electrochemically preparing amorphous elemental selenium film |
-
2017
- 2017-05-23 CN CN201710368088.6A patent/CN107099811A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090283411A1 (en) * | 2008-05-15 | 2009-11-19 | Serdar Aksu | Selenium electroplating chemistries and methods |
| CN101759159A (en) * | 2009-12-24 | 2010-06-30 | 暨南大学 | Method for manufacturing nano-selenium in liquid phase and obtained nano-selenium thereof |
| CN105420779A (en) * | 2015-12-03 | 2016-03-23 | 西南石油大学 | Method for electrochemically preparing amorphous elemental selenium film |
Non-Patent Citations (2)
| Title |
|---|
| QING LI ET AL.，: ""High-yield synthesis of selenium nanowires in water at room temperatue"", 《CHEMCOMM》 * |
| 窦英 等，: "《大学化学实验 无机及分析化学实验分册 （第2版）》", 31 August 2015, 天津大学出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110801438A (en) * | 2019-12-07 | 2020-02-18 | 安徽克菱保健科技有限公司 | Nano-selenium effervescent tablet and preparation method thereof |
| CN112813449A (en) * | 2020-12-31 | 2021-05-18 | 有研国晶辉新材料有限公司 | Method for preparing hydrogen selenide by continuously electrolyzing selenious acid |
| CN112853376A (en) * | 2020-12-31 | 2021-05-28 | 有研国晶辉新材料有限公司 | Method for preparing hydrogen selenide by membrane electrode method |
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