CN105908258A - Preparation method of doped single crystal SnSe - Google Patents
Preparation method of doped single crystal SnSe Download PDFInfo
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- CN105908258A CN105908258A CN201610479617.5A CN201610479617A CN105908258A CN 105908258 A CN105908258 A CN 105908258A CN 201610479617 A CN201610479617 A CN 201610479617A CN 105908258 A CN105908258 A CN 105908258A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention discloses a preparation method of a doped single crystal SnSe. The method comprises the following steps: sealing prepared raw materials into a quartz tube and putting the quartz tube into a furnace with a temperature gradient; raising a furnace temperature to a certain temperature; keeping the heat at the temperature for a period of time and sufficiently fusing the raw materials; and slowly crystallizing the fused raw materials from one end by adopting a Bridgman method and utilizing the temperature gradient in the furnace and a relative position change between a furnace cavity and the raw materials, so as to finally prepare the doped SnSe single crystal. The doped SnSe single crystal prepared by the invention is large in size and excellent in thermoelectric performance; a low-temperature-region ZT value is improved by near one order of magnitude relative to an undoped sample; and the preparation method has the advantages of low raw material cost and environmental friendliness so that the preparation method has a very good actual application prospect.
Description
Technical field
The invention belongs to single crystal preparation technical field, particularly relate to the preparation method of a kind of doped single crystal SnSe.
Background technology
The development of human society is along with the increase of energy resource consumption, and Fossil fuel is as non-renewable energy resources positive day
Benefit reduces, and oneself becomes the popular problem of 21 century to develop new regenerative resource.Thermoelectric material (thermoelectric material)
It is a kind of to utilize transporting and interacting of carrier and phonon in solid, realizes between heat energy and electric energy straight
Connect the functional material of mutually conversion.The thermo-electric generation made by thermoelectric material and refrigeration device have pollution-free,
Noiseless, without abrasion, volume is little, reaction is fast, be easily maintained, the advantage such as safe and reliable, has the most extensive
Application prospect.In addition, thermoelectric generation technology can greatly solve as a kind of novel clean energy technology
The problem of environmental pollution of facing mankind, is especially applied to the utilization of industrial waste heat and answering of sunlight heat
Close generating, for improve the energy utilization rate, develop a circular economy, build a conservation-minded society significant.
But thermoelectric material common problem is that its thermoelectric figure of merit ZT is the highest at present.Property to thermoelectric material
Can be optimized is a kind of important means improving its energy conversion efficiency.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of doped single crystal SnSe, it is intended to solve current thermoelectricity
It is the highest generally to there is its thermoelectric figure of merit ZT in material, and the cost of raw material is high, the problem that energy conversion efficiency is undesirable.
The present invention is achieved in that
The preparation method of a kind of SnSe monocrystalline that adulterates, the preparation method of this doping SnSe monocrystalline includes following step
Rapid:
Step one, prepares and be enclosed in raw material according to certain proportioning raw materials in quartz ampoule, is placed in for sample raw
In long stove；
Step 2, is warming up to uniform temperature by stove, and is incubated a period of time and ensures that raw material fully melts；
Step 3, uses Bu Lijimanfa, and utilize between the thermograde in stove and furnace chamber with raw material is relative
Change in location, makes fused raw material slowly crystallize from one end and finally prepares doping SnSe monocrystalline.
Further, in described step one, raw material is Sn, Se, R, and raw material is that the R in Sn, Se, R is for first
A kind of element in addition to Sn, Se and inert gas elements or the combination of multiple element in element periodic chart.
Further, in described step one, raw material proportioning by mol is:
Sn:R:Se=50～99.9:0.1～50:90～110, proportioning is the most by mol
Sn:R:Se=95～99.9:0.1～5:95～105.
Further, when raw material is enclosed in quartz ampoule by described step one, in quartz ampoule or vacuum state or lazy
Property gas shield state；During vacuum state, vacuum is 10-7～104Pa, during inert gas shielding state, pressure is
10-4～105Pa。
Further, for the stove of sample grown in described step one, for Muffle furnace, tube furnace, shaft furnace
Or a kind of in single crystal growing furnace and there is the stove of thermograde.
Further, in described step 2, stove is raised to temperature and the temperature kept are 700～1200 to take the photograph
Family name's degree, preferable temperature is 870 degrees Celsius～1100 degrees Celsius；Described temperature retention time is 0～100 hour, preferably
Temperature retention time is 0.5～5 hour.
Further, in described step 3, Bu Lijimanfa is a kind of to utilize thermograde to make the solid-liquid of sample divide
Boundary line slowly moves, thus promotes sample method of gradually condensation-crystallization from one end to other end.
Further, in described step 3, in-furnace temperature gradient is 0.01～50 degree/centimetre, and preferred temperature gradient is
0.2～5 degree/centimetre.
Further, in described step 3, relative change in location method between furnace chamber with raw material is: pass through furnace chamber
It is moved away between displacement or raw material displacement or furnace chamber and raw material.
Further, displacement speed is 0.01～100mm/ hour, and preferably translational speed is 0.5～10mm/
Hour.
The doped single crystal SnSe that the present invention provides has the most superior thermoelectricity capability, i.e. has outstanding thermoelectricity
The figure of merit and outstanding average thermoelectric figure of merit, the monocrystalline that the present invention prepares, can be by entirety compared with undoped p monocrystalline
Performance improves 3-6 times, and Material growth required time is quite (big with other traditional polycrystalline thermoelectric materials
About one week), overall thermal electrical property is also top, and the doped single crystal SnSe material that the present invention prepares is available
In the range of average thermoelectric figure of merit ZT there is superiority；The doping SnSe monocrystalline size that the present invention provides is big, heat
Superior electrical property, its low-temperature space ZT value improves a nearly magnitude relative to unadulterated sample.
The present invention optimizes the thermoelectric figure of merit ZT of the carrier concentration raising SnSe material of material by doping, and leads to
Cross crystal growth and realize the acquisition of SnSe height thermoelectricity capability sample, thus be the thermo-electric device system of SnSe material
Standby and actual application lays the first stone；The doping SnSe single crystal samples obtained by this invention shows the most outstanding
Thermoelectricity capability, and its cost of raw material is low, environmental friendliness, thus has good actual application prospect.
Accompanying drawing explanation
Fig. 1 is the preparation method flow chart of the doped single crystal SnSe that the present invention provides.
Fig. 2 is thermoelectricity capability (thermoelectric figure of merit ZT) figure that the present invention provides.
Fig. 3 is doped single crystal SnSe material prepared by the preparation method of the doped single crystal SnSe that the present invention provides
Overall performance curve chart.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment,
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to
Explain the present invention, be not intended to limit the present invention.
Below in conjunction with the accompanying drawings the application principle of the present invention is further described.
As shown in Figure 1:
The preparation method of a kind of SnSe monocrystalline that adulterates, the preparation method of this doping SnSe monocrystalline includes following step
Rapid:
S101: raw material is prepared and is enclosed according to certain proportioning raw materials in quartz ampoule, is placed in for sample raw
In long stove；
S102: stove is warming up to uniform temperature, and be incubated a period of time and ensure that raw material fully melts；
S103: use Bu Lijimanfa, utilize the phase para-position between the thermograde in stove and furnace chamber with raw material
Put change, make fused raw material slowly crystallize from one end and finally prepare doping SnSe monocrystalline.
In described S101, raw material is Sn, Se, R, except Sn, Se and lazy during wherein R is the periodic table of elements
A kind of element beyond property elemental gas or the combination of multiple element.
In described S101, raw material proportioning by mol is: Sn:R:Se=50～99.9:0.1～50:90～110, preferably presses
Mole meter proportioning be Sn:R:Se=95～99.9:0.1～5:95～105.
When raw material is enclosed in quartz ampoule by described S101, in quartz ampoule or vacuum state or inert gas shielding
State；During vacuum state, vacuum is 10-7～104Pa, during inert gas shielding state, pressure is 10-4～105Pa。
For the stove of sample grown in described S101, for Muffle furnace, tube furnace, shaft furnace or single crystal growing furnace
In a kind of and there is the stove of thermograde.
Temperature that in described S102, stove is raised to and the temperature kept are 700～1200 degrees Celsius, excellent
Selecting temperature is 870 degrees Celsius～1100 degrees Celsius；Described temperature retention time is 0～100 hour, preferably temperature retention time
It it is 0.5～5 hour.
In described S103, Bu Lijimanfa is a kind of to utilize thermograde slow to the solid-liquid demarcation line making sample
Mobile, thus promote sample method of gradually condensation-crystallization from one end to other end.
In described S103, in-furnace temperature gradient is 0.01～50 degree/centimetre, preferred temperature gradient is 0.2～5 degree/
Centimetre.
In described S103, the relative change in location method between furnace chamber with raw material is: by furnace chamber displacement or
It is moved away between raw material displacement or furnace chamber and raw material.
Displacement speed is 0.01～100mm/ hour, and preferably translational speed is 0.5～10mm/ hour.
Fig. 2 is that the thermoelectric figure of merit ZT figure that the present invention provides (is by this shown in filled triangle symbols in figure
Bright obtained SnSe single crystal samples).Compared with the classic thermoelectric material being currently known, system of the present invention
Standby doped single crystal material ZT value in whole warm area has shown original；Doping the most involved in the present invention
Its raw material of SnSe is the abundantest in the earth's crust, thus its cost of material is low, and the best in terms of environmental friendliness
In the thermoelectric material that other is leaded.
Fig. 3 is doped single crystal SnSe material prepared by the preparation method of the doped single crystal SnSe that the present invention provides
Overall performance curve chart (figure is shown in filled triangle symbols by the SnSe monocrystalline obtained by the present invention
Sample), overall performance can be improved 3-6 times.
Big with doped single crystal SnSe scantling prepared by the method for the invention, have in available temperature range
Having the most superior thermoelectricity capability, low-temperature space ZT value improves a nearly magnitude relative to unadulterated sample；Material
Material growth required time is suitable with other traditional polycrystalline thermoelectric materials.
The present invention optimizes the thermoelectric figure of merit ZT of the carrier concentration raising SnSe material of material by doping, and leads to
Cross crystal growth and realize the acquisition of SnSe height thermoelectricity capability sample, thus be the thermo-electric device system of SnSe material
Standby and actual application lays the first stone；The doping SnSe single crystal samples obtained by this invention shows the most outstanding
Thermoelectricity capability, and its cost of raw material is low, environmental friendliness, thus has good actual application prospect.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this
Any amendment, equivalent and the improvement etc. made within bright spirit and principle, should be included in the present invention
Protection domain within.
Claims (10)
1. the preparation method of the SnSe monocrystalline that adulterates, it is characterised in that the preparation of this doping SnSe monocrystalline
Method comprises the following steps:
Step one, prepares and be enclosed in raw material according to certain proportioning raw materials in quartz ampoule, is placed in for sample raw
In long stove；
Step 2, is warming up to uniform temperature by stove, and is incubated a period of time and ensures that raw material fully melts；
Step 3, uses Bu Lijimanfa, and utilize between the thermograde in stove and furnace chamber with raw material is relative
Change in location, makes fused raw material slowly crystallize from one end and finally prepares doping SnSe monocrystalline.
2. the preparation method of the SnSe monocrystalline that adulterates as claimed in claim 1, it is characterised in that described step
In rapid one, raw material is Sn, Se, R, raw material be the R in Sn, Se, R be except Sn, Se in the periodic table of elements
And a kind of element beyond inert gas elements or the combination of multiple element.
3. the preparation method of the SnSe monocrystalline that adulterates as claimed in claim 1, it is characterised in that described step
In rapid one, raw material proportioning by mol is: Sn:R:Se=50～99.9:0.1～50:90～110, the most by mol proportioning
For Sn:R:Se=95～99.9:0.1～5:95～105.
4. the preparation method of the SnSe monocrystalline that adulterates as claimed in claim 1, it is characterised in that described step
When raw material being enclosed in quartz ampoule in rapid one, in quartz ampoule or vacuum state or inert gas shielding state；Very
During dummy status, vacuum is 10-7～104Pa, during inert gas shielding state, pressure is 10-4～105Pa。
5. the preparation method of the SnSe monocrystalline that adulterates as claimed in claim 1, it is characterised in that described step
For the stove of sample grown in rapid one, for the one in Muffle furnace, tube furnace, shaft furnace or single crystal growing furnace
And there is the stove of thermograde.
6. the preparation method of the SnSe monocrystalline that adulterates as claimed in claim 1, it is characterised in that described step
Temperature that in rapid two, stove is raised to and the temperature kept are 700～1200 degrees Celsius, and preferable temperature is 870
Degree Celsius～1100 degrees Celsius；Described temperature retention time is 0～100 hour, and preferably temperature retention time is 0.5～5 hour.
7. the preparation method of doped single crystal SnSe as claimed in claim 1, it is characterised in that described step
In rapid three, Bu Lijimanfa is: utilizes thermograde to make the solid-liquid demarcation line of sample slowly move, thus promotes
Sample gradually condensation-crystallization from one end to other end.
8. the preparation method of doped single crystal SnSe as claimed in claim 1, it is characterised in that described step
In rapid three, in-furnace temperature gradient is 0.01 degree Celsius～50 degrees Celsius/centimetre, and preferred temperature gradient is 0.2 Celsius
Degree～5 degrees Celsius/centimetre.
9. the preparation method of doped single crystal SnSe as claimed in claim 1, it is characterised in that described step
In rapid three, the relative change in location method between furnace chamber with raw material is: oriented by furnace chamber displacement or raw material
Move or relative movement between furnace chamber and raw material.
10. displacement as claimed in claim 9, it is characterised in that displacement speed is 0.01mm
～100mm/ hour, preferably translational speed is 0.5mm～10mm/ hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610479617.5A CN105908258A (en) | 2016-06-23 | 2016-06-23 | Preparation method of doped single crystal SnSe |
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| CN201610479617.5A CN105908258A (en) | 2016-06-23 | 2016-06-23 | Preparation method of doped single crystal SnSe |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107400917A (en) * | 2017-07-26 | 2017-11-28 | 武汉理工大学 | A kind of SnSe2Crystalline compounds and its preparation method and application |
| CN107522489A (en) * | 2017-08-23 | 2017-12-29 | 重庆大学 | A kind of preparation method of polycrystalline SnS e thermoelectric materials |
| CN108239787A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院宁波材料技术与工程研究所 | A kind of method for preparing SnSe crystal |
| CN108330543A (en) * | 2018-02-10 | 2018-07-27 | 北京航空航天大学 | A kind of N-type SnSe monocrystalline and preparation method thereof |
| CN108389956A (en) * | 2018-03-09 | 2018-08-10 | 哈尔滨工业大学深圳研究生院 | A kind of preparation method of N-shaped SnSe base Thermoelectric Nano-materials |
| CN108615806A (en) * | 2018-04-26 | 2018-10-02 | 北京航空航天大学 | A kind of N-type SnSe thermoelectric materials and preparation method thereof |
| CN108624958A (en) * | 2018-05-21 | 2018-10-09 | 重庆大学 | A kind of preparation method of doping bulky single crystal SnS |
| CN110129878A (en) * | 2019-05-27 | 2019-08-16 | 南京大学 | A kind of SnSe crystal and its growing method and application with high carrier concentration |
| CN111139519A (en) * | 2020-01-02 | 2020-05-12 | 深圳大学 | Preparation method of flaky SnSe monocrystal |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108239787A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院宁波材料技术与工程研究所 | A kind of method for preparing SnSe crystal |
| CN107400917A (en) * | 2017-07-26 | 2017-11-28 | 武汉理工大学 | A kind of SnSe2Crystalline compounds and its preparation method and application |
| CN107522489A (en) * | 2017-08-23 | 2017-12-29 | 重庆大学 | A kind of preparation method of polycrystalline SnS e thermoelectric materials |
| CN107522489B (en) * | 2017-08-23 | 2020-10-23 | 重庆大学 | Preparation method of polycrystalline SnSe thermoelectric material |
| CN108330543A (en) * | 2018-02-10 | 2018-07-27 | 北京航空航天大学 | A kind of N-type SnSe monocrystalline and preparation method thereof |
| CN108389956A (en) * | 2018-03-09 | 2018-08-10 | 哈尔滨工业大学深圳研究生院 | A kind of preparation method of N-shaped SnSe base Thermoelectric Nano-materials |
| CN108615806A (en) * | 2018-04-26 | 2018-10-02 | 北京航空航天大学 | A kind of N-type SnSe thermoelectric materials and preparation method thereof |
| CN108624958A (en) * | 2018-05-21 | 2018-10-09 | 重庆大学 | A kind of preparation method of doping bulky single crystal SnS |
| CN110129878A (en) * | 2019-05-27 | 2019-08-16 | 南京大学 | A kind of SnSe crystal and its growing method and application with high carrier concentration |
| CN111139519A (en) * | 2020-01-02 | 2020-05-12 | 深圳大学 | Preparation method of flaky SnSe monocrystal |
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Application publication date: 20160831 |