CN106348258A - Preparation method of germanium diselenide powder - Google Patents
Preparation method of germanium diselenide powder Download PDFInfo
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- CN106348258A CN106348258A CN201610796972.5A CN201610796972A CN106348258A CN 106348258 A CN106348258 A CN 106348258A CN 201610796972 A CN201610796972 A CN 201610796972A CN 106348258 A CN106348258 A CN 106348258A
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- germanium
- powder
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- selenium
- germanium selenide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to the technical field of photoelectric material preparation and relates to a powdered material, in particular to a preparation method of germanium diselenide powder. The preparation method includes: evenly mixing germanium powder with selenium powder; performing heating to stay warm under the vacuum condition to complete reaction; when argon gas flows, performing thermal separation and then cooling under argon gas; finally, smashing under protection of the argon gas to obtain the germanium diselenide powder. The germanium diselenide powder is prepared through thermal dispersion reaction of the germanium and the selenium under the high-temperature vacuum; the problem about difficulties in control and purification of the germanium diselenide in reaction of the germanium and the selenium is solved, and the germanium diselenide powder is high in purity; the preparation method is simple, easy to obtain the raw materials, low in energy consumption and convenient in large-scale production.
Description
Technical field
The present invention relates to optoelectronic materials technology, it is related to a kind of dusty material and in particular to a kind of two Germanium selenide powder
Preparation method.
Background technology
, as semi-conducting material, its energy gap is little for two Germanium selenide, all has response to visible ray and near infrared light, it mostly is
Layer structure, in near-infrared photodetection, catalysis etc. is widely used.But about 938.5 DEG C of germanium fusing point, about 2830 DEG C of boiling point,
And the fusing point of selenium is 221 DEG C, boiling point is 684.9 DEG C, because the fusing point of germanium and selenium and boiling point are respectively provided with larger gap, meanwhile, selenium
Easily generate the compound of Germanium selenide and other germanium with the course of reaction of germanium, therefore, both germanium and selenium reaction preparation two Germanium selenide
Reaction is difficult to control, and is more difficult to prepare during its solid state reaction, therefore the research of its domestic and international preparation two Germanium selenide is less, two selenizing germanio
This leans on import, strongly limit application and the development of Germanium selenide.
Content of the invention
The invention aims to solving the above problems, provide a kind of preparation method of two Germanium selenide powder.
In order to reach foregoing invention purpose, the present invention employs the following technical solutions:
A kind of preparation method of two Germanium selenide powder, after the method adopts germanium powder and selenium powder mix homogeneously, first in vacuum condition
Lower heating and thermal insulation, then pulverizes under argon protection and is prepared from.
This case adopts vacuum heat diffusion method, and germanium powder and selenium powder are reacted, thus the two generates the polycrystalline of two Germanium selenide
Product.
Preferably, the mol ratio of the mixed proportion of described germanium powder and selenium powder is 1:2-1:4.
Preferably, described holding temperature is 685-850 DEG C.For holding temperature, germanium is solid, and selenium has arrived at boiling point,
Selenium steam and germanium react, and generate two Germanium selenide of liquid, promote more selenium and germanium to react generation two Germanium selenide.This temperature is very
Important, and the response time want long enough.
Preferably, described temperature retention time is 20-50h.For temperature retention time, the length of temperature retention time and temperature have certain
Contact.Two Germanium selenide and part selenium steam is generated, in order that two Germanium selenide and selenium vapor removal are smoothly, we will be incubated after insulation
Temperature at 685-700 DEG C it is preferred that, and flow and be passed through argon, temperature retention time 15h-30h then natural cooling under argon gas, by
It is 684 DEG C in the boiling point of selenium, and the fusing point of two Germanium selenide is 707 DEG C, in order to ensure that in reaction, unnecessary selenium steam is pulled away, with
When ensure generate two Germanium selenide exist in solid form, therefore temperature is maintained at 685-700 DEG C, according to temperature different choice protect
Difference of warm time.
Preferably, the described rate of heat addition is 5-8 DEG C/min.
Preferably, the method specifically includes following steps:
(1) mol ratio is 1:(2-4) germanium powder and selenium powder, be sufficiently mixed uniformly using agate mortar, then put to quartzy earthenware
In crucible or corundum crucible, finally silica crucible or corundum crucible are put in vacuum drying oven；
(2) to vacuum stove evacuation, and with argon substitution gas more than 10 times, finally make under vacuo very can stove with 5 DEG C/min
Programming rate be warmed up to 660-680 DEG C, and after being incubated 20-50h, natural cooling,；
(3) after completion of the reaction, need 685-700 DEG C of insulation it is preferred that and flow and be passed through argon, temperature retention time 15h-30h,
Separated with two Germanium selenide with inclined selenium steam.
(4) after cooling to room temperature, take out silica crucible or corundum crucible, the red bulk object obtaining is placed into ball
Pulverize in grinding machine, obtain two Germanium selenide powder.
Preferably, the particle diameter of described germanium powder and selenium powder is respectively less than and is equal to 1000 nanometers.
Compared with prior art, beneficial effect is the present invention: the present invention utilizes vacuum heat diffusion method, by germanium under vacuum high-temperature and
The diffusion reaction of selenium, prepares two Germanium selenide powder, and it is more difficult that the present invention solves both germanium and selenium reaction preparation two Germanium selenide
The problem controlling, prepares two higher Germanium selenide powder of purity.Its process is simple, raw material is easy to get, and energy consumption is low, is easy to
A large amount of productions.
Brief description
Fig. 1 is the xrd figure of embodiments of the invention 1 products therefrom；
Fig. 2 is the xrd figure of embodiments of the invention 2 products therefrom.
Specific embodiment
Below by specific embodiment, explanation is further described to technical scheme.
If no specified otherwise, the raw material employed in embodiments of the invention is raw material commonly used in the art, implements
Method employed in example, is the conventional method of this area.
Embodiment 1:
A kind of preparation method of two Germanium selenide powder, after the method adopts germanium powder and selenium powder mix homogeneously, first in vacuum condition
Lower heating and thermal insulation, then when argon flows, is incubated, is then cooled down under argon gas, finally pulverizes system under argon protection
Standby form.
The method specifically includes following steps:
(1) by the germanium powder for 1:2.1 for the mol ratio and selenium powder, it is sufficiently mixed uniformly using agate mortar, then puts to silica crucible
Or in corundum crucible, finally put into silica crucible or corundum crucible in vacuum drying oven；The particle diameter of germanium powder and selenium powder is respectively less than equal to
1000 nanometers；By germanium powder and selenium powder proportionally mix homogeneously；
(2) to vacuum stove evacuation, and with argon substitution gas more than 10 times, finally make under vacuo very can stove with 3 DEG C/min
Programming rate be warmed up to 685 DEG C, and after being incubated 50h, natural cooling；Vacuum starts as 1.35 ~ 25pa, vacuum of then closing the door
Valve, reaction；
(3) after completion of the reaction, it is incubated 700 DEG C, and flows and be passed through argon, temperature retention time 15h, in order to selenium steam and two selenizings
Germanium separates.
(4), under argon protection, after being cooled to room temperature, silica crucible or corundum crucible are taken out, red block by obtain
Object places in ball mill and pulverizes, and obtains two Germanium selenide powder
The xrd figure of preparation-obtained product is shown in Fig. 1.
Knowable to figure, its abscissa is angle, and vertical coordinate is intensity, and it is complete with two Germanium selenide standard card 42-1104
Corresponding, there is no other miscellaneous peaks.Prove preparation for two Germanium selenide powder.
Embodiment 2:
A kind of preparation method of two Germanium selenide powder, after the method adopts germanium powder and selenium powder mix homogeneously, first in vacuum condition
Lower heating and thermal insulation, then when argon flows, is incubated, is then cooled down under argon gas, finally pulverizes system under argon protection
Standby form.
The method specifically includes following steps:
(1) by the germanium powder for 1:4 for the mol ratio and selenium powder, be sufficiently mixed uniformly using agate mortar, then put to silica crucible or
In corundum crucible, finally silica crucible or corundum crucible are put in vacuum drying oven；The particle diameter of germanium powder and selenium powder is respectively less than equal to
1000 nanometers；By germanium powder and selenium powder proportionally mix homogeneously；
(2) to vacuum stove evacuation, and with argon substitution gas more than 10 times, finally make under vacuo very can stove with 3 DEG C/min
Programming rate be warmed up to 685 DEG C, and after being incubated 50h, natural cooling；Vacuum starts as 1.35 ~ 25pa, vacuum of then closing the door
Valve, reaction；
(3) after completion of the reaction, it is incubated 685 DEG C, and flows and be passed through argon, temperature retention time 30h, in order to selenium steam and two selenizings
Germanium separates.
(4), under argon protection, after being cooled to room temperature, silica crucible or corundum crucible are taken out, red block by obtain
Object places in ball mill and pulverizes, and obtains two Germanium selenide powder
The xrd figure of preparation-obtained product is shown in Fig. 2.Understand from figure, its abscissa is angle, vertical coordinate is intensity, itself and selenium
Change germanium standard card 42-1104 completely corresponding, there is no other miscellaneous peaks.Prove preparation for two Germanium selenide powder
Embodiment 3:
A kind of preparation method of two Germanium selenide powder, after the method adopts germanium powder and selenium powder mix homogeneously, first in vacuum condition
Lower heating and thermal insulation, then when argon flows, is incubated, is then cooled down under argon gas, finally pulverizes system under argon protection
Standby form.
(1) by the germanium powder for 1:3 for the mol ratio and selenium powder, it is sufficiently mixed uniformly using agate mortar, then puts to quartzy earthenware
In crucible or corundum crucible, finally silica crucible or corundum crucible are put in vacuum drying oven；The particle diameter of germanium powder and selenium powder be respectively less than etc.
In 1000 nanometers；By germanium powder and selenium powder proportionally mix homogeneously；
(2) to vacuum stove evacuation, and with argon substitution gas more than 10 times, finally make under vacuo very can stove with 3 DEG C/min
Programming rate be warmed up to 800 DEG C, and after being incubated 35h, natural cooling；Vacuum starts as 1.35 ~ 25pa, vacuum of then closing the door
Valve, reaction；
(3) after completion of the reaction, it is incubated 695 DEG C, and flows and be passed through argon, temperature retention time 20h, in order to selenium steam and two selenizings
Germanium separates.
(4), under argon protection, after being cooled to room temperature, silica crucible or corundum crucible are taken out, red block by obtain
Object places in ball mill and pulverizes, and obtains two Germanium selenide powder.
Claims (10)
1. a kind of preparation method of two Germanium selenide powder is it is characterised in that after the method adopts germanium powder and selenium powder mix homogeneously, first
First heating and thermal insulation under vacuum, then pulverizes under argon protection and is prepared from.
2. a kind of preparation method of Germanium selenide powder according to claim 1 is it is characterised in that described germanium powder and selenium powder
The mol ratio of mixed proportion is 1:2-4.
3. a kind of preparation method of two Germanium selenide powder according to claim 1 is it is characterised in that described holding temperature is
685-850℃.
4. a kind of preparation method of the two Germanium selenide powder according to claim 1 or 3 is it is characterised in that during described insulation
Between be 20-50h.
5. a kind of preparation method of the two Germanium selenide powder according to claim 1 or 2 or 3 is it is characterised in that described vacuum
The vacuum that condition is is 1.35 ~ 25pa.
6. a kind of preparation method of two Germanium selenide powder according to claim 5 is it is characterised in that by germanium powder and selenium powder
Proportionally after mix homogeneously, put in quartz or corundum crucible.
7. a kind of preparation method of the Germanium selenide powder according to claim 1 or 2 or 3 or 6 is it is characterised in that described add
Hot speed is 5-8 DEG C/min.
8. a kind of preparation method of two Germanium selenide powder according to claim 1 is it is characterised in that reacted under vacuo
Cheng Hou, needs described holding temperature to be 685-700 DEG C, is incubated 15-30h, so that two Germanium selenide and selenium vapor removal.
9. a kind of Germanium selenide powder according to claim 1 preparation method it is characterised in that the method specifically include with
Lower step:
(1) mol ratio is 1:(2-4) germanium powder and selenium powder, be sufficiently mixed uniformly using agate mortar, then put to quartzy earthenware
In crucible or corundum crucible, finally silica crucible or corundum crucible are put in vacuum drying oven；
(2) to vacuum stove evacuation, and with argon substitution gas more than 10 times, finally make under vacuo very can stove with 5 DEG C/min
Programming rate be warmed up to 685-850 DEG C, and after being incubated 20-50h, after generating two Germanium selenide completely, in the insulation of 685-700 degree
20h, and flow and be passed through argon, then natural cooling under argon gas；
(3), after being cooled to room temperature, open very fast stove and take out silica crucible or corundum crucible, by the pink obtaining or yellow color
Block object places in ball mill and pulverizes, and obtains Germanium selenide powder.
10. a kind of two Germanium selenide powder according to claim 1 or 9 preparation method it is characterised in that described germanium powder and
The particle diameter of selenium powder is respectively less than and is equal to 1um.
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| CN201610796972.5A CN106348258A (en) | 2016-08-31 | 2016-08-31 | Preparation method of germanium diselenide powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109081316A (en) * | 2017-06-13 | 2018-12-25 | 天津大学 | A kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process |
| CN110282975A (en) * | 2019-07-08 | 2019-09-27 | 先导薄膜材料（广东）有限公司 | A kind of Germanium selenide target and preparation method thereof |
| CN114368729A (en) * | 2022-01-13 | 2022-04-19 | 湘潭大学 | GeSe for directional growth2Nanowire and method for preparing same |
| CN115285947A (en) * | 2022-08-12 | 2022-11-04 | 深圳博磊达新能源科技有限公司 | Selenide negative electrode material for sodium ion battery, preparation method of selenide negative electrode material and sodium ion battery |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109081316A (en) * | 2017-06-13 | 2018-12-25 | 天津大学 | A kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process |
| CN110282975A (en) * | 2019-07-08 | 2019-09-27 | 先导薄膜材料（广东）有限公司 | A kind of Germanium selenide target and preparation method thereof |
| CN114368729A (en) * | 2022-01-13 | 2022-04-19 | 湘潭大学 | GeSe for directional growth2Nanowire and method for preparing same |
| CN115285947A (en) * | 2022-08-12 | 2022-11-04 | 深圳博磊达新能源科技有限公司 | Selenide negative electrode material for sodium ion battery, preparation method of selenide negative electrode material and sodium ion battery |
| CN115285947B (en) * | 2022-08-12 | 2023-06-16 | 深圳博磊达新能源科技有限公司 | Selenide anode material for sodium ion battery, preparation method of selenide anode material and sodium ion battery |
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Application publication date: 20170125 |