CN108239787A - A kind of method for preparing SnSe crystal - Google Patents
A kind of method for preparing SnSe crystal Download PDFInfo
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- CN108239787A CN108239787A CN201611226276.7A CN201611226276A CN108239787A CN 108239787 A CN108239787 A CN 108239787A CN 201611226276 A CN201611226276 A CN 201611226276A CN 108239787 A CN108239787 A CN 108239787A
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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Abstract
This application provides a kind of methods for preparing SnSe crystal, which is characterized in that is obtained being grown in the container being placed in italic growth furnace containing SnSe polycrystalline raw materials；The axial angle with horizontal direction of the furnace body of the italic growth furnace is 15~30 °.This method effectively reduces the contact area of crystal and container by using italic growth, and pass through the measures such as smaller temperature gradient, the slower speed of growth and slow crystal cooling rate, reach and suppressed or eliminated the source that crystal growth different phase generates stress, be conducive to obtain high integrality SnSe crystal.
Description
Technical field
This application involves a kind of methods for preparing SnSe crystal, belong to inorganic material synthesis field.
Background technology
With being constantly progressive for industrial level, the whole world also increasingly increases, but this also brings simultaneously the demand of the energy
Serious problem of environmental pollution.Based on this, environmental-friendly regenerative resource research becomes emphasis of concern.Thermoelectric material
It is a kind of functional material that can be realized thermal energy and mutually be converted with electric energy, thermo-electric device can contamination-freely be generated using various heats
Electric energy, such as solar energy, industrial waste heat, CPU dissipate and human body thermoelectric, i.e., simply by the presence of the temperature difference, it is possible to export energy, this is right
Efficiently using for resource can generate far-reaching influence.For a long time, the research hotspot of thermoelectric material is concentrated mainly on alloy and partly leads
The Clathrates that Skutterudites types alloy, Half-Heusler intermetallic compounds, low-heat are led such as is filled in body field
Type alloy, chalcogenide, Nano semiconductor alloy etc..However the relatively low energy conversion efficiency of thermoelectric material is still limit at present
The bottleneck of its application is made, makes it that can only be used under the conditions of small-power.In recent years, a kind of SnSe crystalline materials were because with excellent
Thermoelectricity capability and create much of a stir in the world.SnSe crystal is up to 2.6 at a temperature of 923K along the thermoelectric figure of merit ZT of b axis directions,
This numerical value is unprecedented, is the peak in all thermoelectricity systems, and SnSe monocrystalline also may be used along the thermoelectric figure of merit in c-axis direction
To reach 2.3.The thermoelectric figure of merit of SnSe crystal superelevation mainly has benefited from it with ultralow lattice thermal conductivity, this discovery is broken
Traditional understandings of the people to thermoelectric material provide brand-new Research Thinking for new thermoelectric materials exploration.
However the extremely difficult growth of SnSe crystal, at present in the world mainly using vertical bridgman method (VB), improved vertical
Prepared by Bridgman method (MB), but the SnSe crystal of this technique growth is very easy to crack, and success rate is very low.Cause this
The reason of kind phenomenon, is mainly caused by the special construction of SnSe crystal.SnSe belongs to rhombic system, has layer structure, in b-
In c planes, there is stronger bonding between Sn-Se, form SnSe diatomic plane layers, and along a axis directions, between Sn-Se then
In the presence of weaker active force.Therefore crystal is in growth course, if material internal stress cannot be released effectively or eliminate, SnSe
Crystal is then easily along (100) face cleavatge of crystals, it is difficult to obtain the SnSe crystalline materials of high quality high integrality.
Invention content
According to the one side of the application, a kind of method for preparing SnSe crystal is provided, this method is given birth to by using italic
The long contact area for effectively reducing crystal and container, and pass through smaller temperature gradient, the slower speed of growth and slowly
The measures such as crystal cooling rate have reached and have suppressed or eliminated the source that crystal growth different phase generates stress, have been conducive to obtain
High integrality SnSe crystal.
The method for preparing SnSe crystal, which is characterized in that italic growth furnace will be placed in containing SnSe polycrystalline raw materials
In container in grow and obtain；
The axial angle with horizontal direction of the furnace body of the italic growth furnace is 15~30 °.
Preferably, the italic growth furnace includes high-temperature region, middle warm area and low-temperature space；Wherein, high-temperature region temperature for 900~
950 DEG C, middle warm area temperature is 860~900 DEG C, and low-temperature space temperature is 800~860 DEG C.
It is further preferred that high-temperature region temperature is 910~920 DEG C, middle warm area temperature is 890~895 DEG C, low-temperature space temperature
It is 860~870 DEG C.
Preferably, 60~120 ° of the shouldering angle of the container.
Preferably, a diameter of 2~4 inches of the container.It is further preferred that the container is silica crucible.
As a kind of embodiment of itself, it is equipped with SnSe seed crystals, seed orientation in the container<100>、<110>、<
111>。
As a kind of embodiment of itself, the method for preparing SnSe crystal, including at least following steps：
A) sealed after being vacuumized in crucible will be fitted into containing SnSe polycrystalline raw materials；60~120 ° of crucible shouldering angle, dress
It is oriented to<100>、<110>、<111>Seed crystal；
B) crucible after sealing is placed in italic growth furnace, control italic reacting furnace high temperature area temperature is 900~950
DEG C, middle warm area temperature is 860~900 DEG C, and low-temperature space temperature is 800~860 DEG C of progress crystal growths；The furnace body of italic growth furnace
The axial angle with horizontal direction is 15~30 °；
C) it after the SnSe polycrystalline in raw material all melts and completes inoculation with seed crystal, is slowly dropped with 15~20 DEG C/h speed
To room temperature to get the SnSe monocrystalline.
Preferably, the temperature gradient size of the crystal growth of middle warm area is 3~5 DEG C/cm, and the speed of growth is 0.5~2mm/
h.It is further preferred that SnSe crystal growths mainly carry out in middle warm area T2, the temperature gradient size of crystal growth is 3~5
DEG C/cm, the speed of growth is 0.5~2mm/h, and crystal cooling velocity is 15~20 DEG C/h.
Preferably, the liquid level of SnSe polycrystalline melt is less than silica crucible shouldering and the turning of isometrical transition position.
As a preferred embodiment, the method for preparing SnSe crystal, includes the following steps：
(1) furnace body of italic growth furnace is axial and horizontal direction angle is 15~30 °；
(2) italic growth furnace heating element is entwined by the Fe-Co-Al resistance wires for being resistant to 1280 DEG C of high temperature, and furnace body adds
Heat is divided into 7 sections, is controlled respectively by program；
(3) furnace body thermal field is divided into three warm areas：The high-temperature region T1 that is made of the 1st~3 section of heating element, by the 4th and 5 section plus
The middle warm area T2 that thermal element the is formed and low-temperature space T3 being made of the 6th and 7 section of heating element；
(4) SnSe crystal is grown in silica crucible is sealed, and silica crucible shouldering angle is 60~120 °.
SnSe crystal is mainly grown in middle warm area T2.Container used in SnSe crystal growths for shouldering angle 60~
120 °, the silica crucible of 2~4 inches of diameter.Silica crucible tail portion is equipped with direction<100>、<110>、<111>SnSe seeds
It is brilliant.SnSe crystal growths need to carry out under vacuum, and the pressure in silica crucible is evacuated device and is evacuated to 10-3Pa magnitudes
Afterwards, it is sealed with oxyhydrogen flame.SnSe crystal is grown in silica crucible, and the liquid level of SnSe melts will be less than stone
The shouldering of English crucible and the turning of isometrical transition position.After SnSe melts and SnSe seed crystals fully complete inoculation, SnSe is come into effect
Crystal growth.In order to inhibit to generate thermal stress in crystal growing process, SnSe crystal need to be in smaller temperature gradient and slower
It is carried out under the speed of growth.For the temperature gradient size that the application uses for 3~5 DEG C/cm, the speed of growth is 0.5~2mm/h.SnSe
Melt at the seed crystal inoculation continuous decrease temperature crystalline up to completing, last SnSe crystal is controlled through each section of program, with 15~20
DEG C/h speed is slowly dropped to room temperature.Since SnSe melt liquid levels are low, avoid in crystal temperature-fall period because of coefficient of thermal expansion difference
Caused by extruding of the silica crucible to crystalline material, substantially increase SnSe perfection of crystals.
According to the another aspect of the application, provide a kind of crystal growing furnace, the crystal growing furnace by by tilting furnace extremely
Suitable angle reduces the contact area of crystal and container, suppresses or eliminates crystal growth different phase and generates coming for stress
Source.
The crystal growing furnace includes furnace body, the furnace body support for being used to support the furnace body, the heating unit controlled by program
Part and the burner hearth in the furnace body；The axial angle with horizontal direction of the furnace body is 15~30 °.
As a kind of embodiment, three temperature regions of the burner hearth point：Superposed high-temperature region, in middle part
Warm area, the low-temperature space positioned at lower part.Preferably, the heating element is wound by resistance wire, is divided into seven sections；Wherein, the 1st to
3 sections of corresponding high-temperature regions, the 4th and 5 section of corresponding middle warm area, the 6th and 7 section of corresponding low-temperature space.
Preferably, the resistance wire is the Fe-Co-Al resistance wires for being resistant to 1280 DEG C of high temperature.
The advantageous effect of the application includes but not limited to：
(1) method for preparing SnSe crystal provided herein, by using italic growth effectively reduce crystal with
The contact area of container, and by measures such as smaller temperature gradient, the slower speed of growth and slow crystal cooling rates,
Reach and suppressed or eliminated the source that crystal growth different phase generates stress, obtained high integrality SnSe crystal.
(2) method for preparing SnSe crystal provided herein, in order to control material stress formed and stress elimination in terms of
Provide new way.
(3) crystal growing furnace provided herein, by by tilting furnace to suitable angle, reducing crystal with holding
The contact area of device suppresses or eliminates the source that crystal growth different phase generates stress.
Description of the drawings
Fig. 1 is a kind of schematic diagram of embodiment of the application.
Specific embodiment
The application is described in detail, but the application is not limited to these embodiments with reference to embodiment.
Below in conjunction with Fig. 1, to the application, a kind of specific embodiment is described：
By SnSe polycrystalline be fitted into 60~120 ° of shouldering angle, 2~4 inches of diameter silica crucible in, use hydrogen after vacuumizing
Oxygen flame is sealed；Silica crucible tail portion is equipped with and is oriented to<100>、<110>、<111>Seed crystal；Crucible after sealing is put
In italic growth furnace, the axial angle with horizontal direction of furnace body of italic growth furnace is 15~30 °；Control italic reacting furnace
Heating element is entwined by the Fe-Co-Al resistance wires for being resistant to 1280 DEG C of high temperature, and furnace body heating is divided into 7 sections, respectively by program control
System, corresponding three warm areas：Corresponding 900~950 DEG C of high-temperature regions of 1st~3 section of heating element, the 4th and 5 section of heating element are corresponding
860~900 DEG C of middle warm areas and corresponding 800~860 DEG C of low-temperature spaces of the 6th and 7 section of heating element；SnSe crystal is in silica crucible
It is grown, the liquid level of SnSe melts will be less than silica crucible shouldering and the turning of isometrical transition position, temperature gradient size
For 3~5 DEG C/cm, the speed of growth is 0.5~2mm/h.After SnSe melts and SnSe seed crystals fully complete inoculation, come into effect
SnSe crystal growths.SnSe melts at the seed crystal inoculation continuous decrease temperature crystalline up to completing, last SnSe crystal is through each section
Program controls, and room temperature is slowly dropped to get the SnSe crystal with 15~20 DEG C/h speed.
Embodiment 1
1 kilogram of SnSe polycrystal material is fitted into the silica crucible of 2 inches diameter, silica crucible shouldering angle is 90 °, is taken out true
Sky is to 1.5 × 10-3Pa is simultaneously sealed with oxyhydrogen flame.Silica crucible is placed in italic growth furnace 1,1 axial direction of italic growth furnace and water
Flat angular separation is 15 °.The T1 temperature control of furnace high-temperature area is 920 DEG C, and the control of middle warm area T2 temperature is 890 DEG C, low-temperature space T3
Temperature control is 860 DEG C.After SnSe polycrystal materials all melt and complete inoculation with (100) SnSe seed crystals in silica crucible,
SnSe crystal carries out growth until all crystallizations of SnSe melts, last SnSe crystal with 5 DEG C/cm temperature gradients, 0.8mm/h speed
Room temperature is down to 15 DEG C/h speed, obtains high integrality SnSe crystal.
Embodiment 2：
1.5 kilograms of SnSe polycrystal materials being fitted into the silica crucible of 3 inches of diameter, silica crucible shouldering angle is 100 °,
It is evacuated to 1.2 × 10-3Pa is simultaneously sealed with oxyhydrogen flame.Silica crucible is placed in italic growth furnace, italic growth furnace 1 it is axial with
Horizontal direction angle is 20 °.The T1 temperature control of furnace high-temperature area is 910 DEG C, and the control of middle warm area T2 temperature is 895 DEG C, low-temperature space
The control of T3 temperature is 870 DEG C.Treat that SnSe polycrystal materials all melt and complete to be inoculated with (110) SnSe seed crystals in silica crucible
Afterwards, SnSe crystal carries out growth until all crystallizations of SnSe melts, last SnSe with 4 DEG C/cm temperature gradients, 1.2mm/h speed
Crystal is down to room temperature with 18 DEG C/h speed, obtains high integrality SnSe crystal.
Embodiment 3：
1.8 kilograms of SnSe polycrystal materials being fitted into the silica crucible of 4 inches of diameter, silica crucible shouldering angle is 100 °,
It is evacuated to 1.8 × 10-3Pa is simultaneously sealed with oxyhydrogen flame.Silica crucible is placed in italic growth furnace, italic growth furnace it is axial with
Horizontal direction angle is 25 °.The T1 temperature control of furnace high-temperature area is 910 DEG C, and the control of middle warm area T2 temperature is 890 DEG C, low-temperature space
The control of T3 temperature is 870 DEG C.Treat that SnSe polycrystal materials all melt and complete to be inoculated with (111) SnSe seed crystals in silica crucible
Afterwards, SnSe crystal carries out growth until all crystallizations of SnSe melts, last SnSe with 3 DEG C/cm temperature gradients, 1.5mm/h speed
Crystal is down to room temperature with 18 DEG C/h speed, obtains high integrality SnSe crystal.
Embodiment 4：
2 kilograms of SnSe polycrystal materials are fitted into the silica crucible of 4 inches of diameter, silica crucible shouldering angle is 120 °, is taken out
Vacuum is to 2 × 10-3Pa is simultaneously sealed with oxyhydrogen flame.Silica crucible is placed in italic growth furnace 1,1 axial direction of italic growth furnace and water
Flat angular separation is 30 °.The T1 temperature control of furnace high-temperature area is 915 DEG C, and the control of middle warm area T2 temperature is 890 DEG C, low-temperature space T3
Temperature control is 865 DEG C.After SnSe polycrystal materials all melt and complete inoculation with (111) SnSe seed crystals in silica crucible,
SnSe crystal with 3 DEG C/cm temperature gradients, 2mm/h speed carry out growth until SnSe melts all crystallize, last SnSe crystal with
20 DEG C/h speed is down to room temperature, obtains high integrality SnSe crystal.
The above is only several embodiments of the application, any type of limitation is not done to the application, although this Shen
Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off
In the range of technical scheme, make a little variation using the technology contents of the disclosure above or modification is equal to
Case study on implementation is imitated, is belonged in the range of technical solution.
Claims (10)
- A kind of 1. method for preparing SnSe crystal, which is characterized in that will be placed in italic growth furnace containing SnSe polycrystalline raw materials Container in grow and obtain；The axial angle with horizontal direction of the furnace body of the italic growth furnace is 15~30 °.
- 2. according to the method described in claim 1, it is characterized in that, the italic growth furnace includes high-temperature region, middle warm area and low Warm area；Wherein, high-temperature region temperature is 900~950 DEG C, and middle warm area temperature is 860~900 DEG C, and low-temperature space temperature is 800~860 ℃。
- 3. according to the method described in claim 1, it is characterized in that, 60~120 ° of the shouldering angle of the container.
- 4. the method according to claim 1 or 3, which is characterized in that the container is the silica crucible of 2~4 inches of diameter.
- 5. according to the method described in claim 1, it is characterized in that, it is equipped with SnSe seed crystals, seed orientation in the container< 100>、<110>、<111>。
- 6. according to the method described in claim 1, it is characterized in that, including at least following steps：A) sealed after being vacuumized in crucible will be fitted into containing SnSe polycrystalline raw materials；60~120 ° of crucible shouldering angle, equipped with taking Xiang Wei<100>、<110>、<111>Seed crystal；B) crucible after sealing being placed in italic growth furnace, control italic reacting furnace high temperature area temperature is 900~950 DEG C, Middle warm area temperature is 860~900 DEG C, and low-temperature space temperature is 800~860 DEG C of progress crystal growths；The furnace body axis of italic growth furnace It it is 15~30 ° to the angle with horizontal direction；C) after the SnSe polycrystalline in raw material all melts and completes inoculation with seed crystal, room is slowly dropped to 15~20 DEG C/h speed Temperature is to get the SnSe crystal.
- 7. the method according to claim 2 or 6, which is characterized in that the temperature gradient size of the crystal growth of middle warm area is 3 ~5 DEG C/cm, the speed of growth is 0.5~2mm/h.
- 8. a kind of crystal growing furnace, including furnace body, the furnace body support that is used to support the furnace body, the heating element controlled by program And the burner hearth in the furnace body；The axial angle with horizontal direction of the furnace body is 15~30 °.
- 9. crystal growing furnace according to claim 8, which is characterized in that three temperature regions of the burner hearth point：Positioned at upper The high-temperature region in portion, the middle warm area positioned at middle part, the low-temperature space positioned at lower part.
- 10. crystal growing furnace according to claim 9, which is characterized in that the heating element is wound by resistance wire, It is divided into seven sections；Wherein, the 1st to 3 section of corresponding high-temperature region, the 4th and 5 section of corresponding middle warm area, the 6th and 7 section of corresponding low-temperature space.
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| CN201611226276.7A CN108239787A (en) | 2016-12-27 | 2016-12-27 | A kind of method for preparing SnSe crystal |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161970A (en) * | 2018-10-11 | 2019-01-08 | 哈尔滨工业大学 | A kind of visual three-temperature-zone gallium selenide single-crystal growing apparatus and growing method |
| 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 |
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| CN1594672A (en) * | 2004-06-30 | 2005-03-16 | 哈尔滨工业大学 | Visual temperature ladder crystal condensation growth device with low oblique and growth method thereof |
| CN105399061A (en) * | 2015-11-18 | 2016-03-16 | 山东师范大学 | Preparation method for one-dimensional SnSe monocrystal nanowire |
| CN105908258A (en) * | 2016-06-23 | 2016-08-31 | 重庆大学 | Preparation method of doped single crystal SnSe |
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| CN1594672A (en) * | 2004-06-30 | 2005-03-16 | 哈尔滨工业大学 | Visual temperature ladder crystal condensation growth device with low oblique and growth method thereof |
| CN105399061A (en) * | 2015-11-18 | 2016-03-16 | 山东师范大学 | Preparation method for one-dimensional SnSe monocrystal nanowire |
| CN105908258A (en) * | 2016-06-23 | 2016-08-31 | 重庆大学 | Preparation method of doped single crystal SnSe |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161970A (en) * | 2018-10-11 | 2019-01-08 | 哈尔滨工业大学 | A kind of visual three-temperature-zone gallium selenide single-crystal growing apparatus and growing method |
| CN109161970B (en) * | 2018-10-11 | 2021-04-06 | 哈尔滨工业大学 | Visible three-temperature-zone gallium selenide single crystal growth device and growth method |
| 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 |
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Application publication date: 20180703 |