CN108615806B - A kind of N-type SnSe thermoelectric material and preparation method thereof - Google Patents
A kind of N-type SnSe thermoelectric material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of N-type SnSe thermoelectric materials, belong to technical field of energy material, and the N-type SnSe thermoelectric material is made of Sn, Se and Br atom, and the atomic molar ratio of described Sn, Se and Br are 1:0.97~0.99:0.01~0.03；The N-type SnSe thermoelectric material is monocrystalline, and the cell parameter abc of the crystal is respectivelyShaft angle α, β, γ are 90 °；The ZT value of the N-type SnSe thermoelectric material is 2.0~2.8.The N-type SnSe thermoelectric material that the present invention obtains is monocrystalline, eliminates the influence of crystal boundary and impurity to electron-transport, so that electrical property is significantly improved, realizes the raising of the n type material component thermoelectricity capability of the thermo-electric device based on SnSe crystal.
Description
Technical field
The present invention relates to technical field of energy material more particularly to a kind of N-type SnSe thermoelectric material and preparation method thereof.
Background technique
Thermoelectric energy conversion technology is a kind of technology for directly mutually being converted thermal energy and electric energy using functional material.
One basic thermoelectric power generation unit is put in parallel by a p-type thermoelectric semiconductor material and a N-type thermoelectric semiconductor material
It sets, PN type material ends is then welded together into composition with conductive module.And the component of thermoelectric power generation is by a large amount of base
This thermoelectric power generation unit is constituted in electrical series calorifics parallel connection.Thermoelectric components energy conversion efficiency is by component temperature difference between the two ends and warm
The performance figure of merit ZT of electric material is determined.When temperature-resistant, performance figure of merit ZT is higher, and the energy conversion efficiency of thermoelectric components is got over
It is high.
SnSe is a kind of important thermoelectricity energy and material, is a kind of with extremely strong anisotropic stratified material, edge
In layer direction there is high carrier mobility, and perpendicular layers direction has low thermal conductivity.Prepare high-performance SnSe thermoelectricity
Material is most important for thermoelectricity energy research.Before, people successfully have developed high performance p-type SnSe thermoelectric material.For example,
Low-heat is caused to lead undoped p-type stannic selenide crystal SnSe [Zhao, the L.D. of effect using using Non-resonance effect；Lo,S.H.；
Zhang,Y.；Sun,H.；Tan,G.；Uher,C.；Wolverton,C.；Dravid,V.P.；Kanatzidis,M.G.,
Ultralow thermal conductivity and high thermoelectric figure of merit in SnSe
crystals.Nature 2014,508(7496),373-7.]；It is adulterated using Alkali-Metal Na and improves carrier concentration and plug shellfish
P-type natrium doping SnSe crystal [Zhao, the L.D. of gram coefficient；Tan,G.；Hao,S.；He,J.；Pei,Y.；Chi,H.；Wang,
H.；Gong,S.；Xu,H.；Dravid,V.P.；Uher,C.；Snyder,G.J.；Wolverton,C.；Kanatzidis,
M.G.,Ultrahigh power factor and thermoelectric performance in hole-doped
single-crystal SnSe.Science 2016,351(6269),141-4.]。
The P-type crystal SnSe of above method preparation has very high ZT value.But a high-performance thermo-electric device must be same
When p-type and N-type component with Performance Match, therefore it is very necessary to find a kind of high-performance N-type SnSe thermoelectric material.Existing skill
The customary preparation methods of art N-type SnSe have melt-synthesizing+discharge plasma sintering and high-energy ball milling method, their defect is
Preparation is polycrystalline SnS e, and a large amount of crystal boundary and defect of introducing hinder the transmission of electronics, reduce conductivity.
Summary of the invention
In view of this, the present invention provides a kind of N-type SnSe thermoelectric material and preparation method thereof, SnSe provided by the invention
Thermoelectric material is monocrystalline, eliminates the influence of crystal boundary and impurity to electron-transport, so that electrical property is significantly improved, is realized
The raising of the n type material component thermoelectricity capability of thermo-electric device based on SnSe crystal.
The present invention provides a kind of N-type SnSe thermoelectric material, the N-type SnSe thermoelectric material is by Sn, Se and Br atom group
At the atomic molar ratio of described Sn, Se and Br are 1:0.97~0.99:0.01~0.03；The N-type SnSe thermoelectric material is single
The cell parameter a b c of crystalline substance, the crystal is respectivelyShaft angle α, β,
γ is 90 °；The ZT value of the N-type SnSe thermoelectric material is 2.0~2.8.
The present invention also provides the preparation methods of the N-type SnSe thermoelectric material, comprising the following steps:
By Sn, Se and SnBr2It is mixed to get mixed material, the atomic molar ratio of Sn, Se and Br are in the mixed material
1:0.97~0.99:0.01~0.03；
The mixed material is synthesized into N-type SnSe thermoelectric material according to vertical gradient dual temperature area's cooling method.
Preferably, the quality purity of the Sn and Se is independently greater than 99.99%, the SnBr2Quality purity be greater than
99%.
Preferably, vertical gradient dual temperature area's cooling method the following steps are included:
1) mixed material is put into low side is to carry out vacuumize process in the quartz ampoule of taper and angle less than 30 °；
2) gained in the step 1) is placed in dual temperature area vertical tube furnace equipped with the quartz ampoule of mixed material, is closed
At reaction, N-type SnSe thermoelectric material is obtained.
Preferably, the vacuum degree in the step 1) after vacuumize process is less than 10-3Pa。
Preferably, the material upper end horizontal position of the quartz ampoule in the step 2) equipped with mixed material is located at warm area thermoelectricity
Even horizontal position, the low side tip of the quartz ampoule equipped with mixed material are located at below warm area thermocouple horizontal position at 5cm.
Preferably, in the step 2) the upper warm area of dual temperature area vertical tube furnace temperature control program are as follows: be first warming up to 1050
DEG C, 600min is kept the temperature, first is then carried out and is cooled to 800 DEG C, then carry out second and be cooled to 25 DEG C.
Preferably, the heating rate of the warm area independently is 50 DEG C/h~100 DEG C/h, the cooling speed of first cooling
Rate is 1 DEG C/h, and the rate of temperature fall of second cooling is 20 DEG C/h.
Advantageous effects: N-type SnSe thermoelectric material provided by the invention is monocrystalline, eliminates crystal boundary and impurity to electronics
The influence of transmission realizes the n type material component of the thermo-electric device based on SnSe crystal so that electrical property is significantly improved
The raising of thermoelectricity capability.Specific embodiment shows the most high zt of N-type SnSe thermoelectric material provided by the invention 2.0~2.8
Between.
Detailed description of the invention:
Fig. 1 is the structural schematic diagram of dual temperature area vertical tube furnace of the invention；
Fig. 2 is the cut direction schematic diagram of N-type SnSe thermoelectric material in embodiment 1；
Fig. 3 is the Laue diffraction pattern spectrum for applying the crystal dissociation face of N-type SnSe thermoelectric material in example 1；
Fig. 4 is the thermoelectricity capability test chart that the samples vertical after cutting in Examples 1 to 5 is carried out in dissociation face direction.
Specific embodiment
The present invention provides a kind of N-type SnSe thermoelectric material, the N-type SnSe thermoelectric material is by Sn, Se and Br atom group
At the atomic molar ratio of described Sn, Se and Br are 1:0.97~0.99:0.01~0.03；The N-type SnSe thermoelectric material is single
The cell parameter a b c of crystalline substance, the crystal is respectivelyShaft angle α, β,
γ is 90 °；The ZT value of the N-type SnSe thermoelectric material is 2.0~2.8.
In the present invention, the atomic molar of described Sn, Se and Br are than being preferably 1:0.98:0.02.
In the present invention, the ZT value of the N-type SnSe thermoelectric material is preferably 2.3~2.8.
The present invention also provides the preparation methods of the N-type SnSe thermoelectric material, comprising the following steps:
By Sn, Se and SnBr2Mixing, obtains mixed material, the atomic molar ratio of Sn, Se and Br are in the mixed material
1:0.97~0.99:0.01~0.03；
The mixed material is synthesized into N-type SnSe thermoelectric material according to vertical gradient dual temperature area's cooling method.
The present invention is by Sn, Se and SnBr2It is mixed to get mixed material, the atom of Sn, Se and Br rub in the mixed material
You are than being 1:0.97~0.99:0.01~0.03.
In the present invention, the quality purity of the Sn and Se is independently preferably greater than 99.99%, the SnBr2Matter
Measuring purity is preferably greater than 99%.
In the present invention, the atomic molar ratio of Sn, Se and Br are preferably 1:0.98:0.02 in the mixed material.It is adopting
With in preparation process of the invention, the SnBr2As doped chemical, intrinsic SnSe can be made to become N-type SnSe.
After obtaining mixed material, the mixed material is synthesized N-type according to vertical gradient dual temperature area's cooling method by the present invention
SnSe thermoelectric material.
In the present invention, vertical gradient dual temperature area cooling method preferably includes following steps:
1) mixed material is put into quartz ampoule, carries out vacuumize process；
2) gained in the step 1) is placed in dual temperature area vertical tube furnace equipped with the quartz ampoule of mixed material, is closed
At reaction, N-type SnSe thermoelectric material is obtained.
The mixed material is put into quartz ampoule by the present invention, carries out vacuumize process.
In the present invention, the vacuum degree after the vacuumize process is preferably smaller than 10-3Pa, it is in the present invention, described to take out very
Vacancy reason preferably includes successively to carry out the first vacuumize process and the second vacuumize process；First vacuumize process preferably will
Quartz ampoule is evacuated to vacuum degree less than 10-2Pa, second vacuumize process are by the quartz ampoule after the first vacuumize process
Vacuum degree is evacuated to less than 10-3Pa.In the present invention, quartz ampoule is evacuated to vacuum degree less than 10-3Pa can be prevented
Raw material aoxidizes in single crystal growth process.
In the present invention, first vacuumize process preferably includes to vacuumize-inflation cycle process, it is described vacuumize-
Inflation cycle process preferably carries out 3 times or more.In an embodiment of the present invention, the inflation is specially filled in quartz ampoule lazy
Property gas.The present invention using vacuumize-inflation cycle process can sufficiently exclude air in tank body.
After completing first vacuumize process, the present invention preferably carries out the second vacuumize process.Described second is completed to take out
After vacuum processing, gained quartz ampoule is preferably sealed processing by the present invention.The present invention does not have the method for the encapsulation process
There is special restriction, using the method for sealed silica envelope well known to those skilled in the art.In specific implementation of the invention
In example, flame sealed silica envelope is specifically used.
After completing the vacuumize process, gained is placed in dual temperature area vertical tube equipped with the quartz ampoule of mixed material by the present invention
In formula furnace, synthetic reaction is carried out, N-type SnSe thermoelectric material is obtained.SnSe is during cooling solidification due to phase transformation in order to prevent
Crack quartz ampoule and contacted with air and aoxidized, the present invention preferably by after the vacuumize process quartz ampoule (small quartz ampoule, directly
Diameter is placed in outer layer quartz ampoule (big quartz ampoule, diameter are greater than small quartz ampoule) for 5mm, 10mm or 15mm) and synthesize instead
It answers.Size of the present invention using the internal diameter control product of small quartz ampoule, size and the small quartz ampoule of gained SnSe single crystal product article
Internal diameter is identical.In an embodiment of the present invention, it specifically, being put into mixed material in small quartz ampoule, is vacuumized
Gained is placed in big quartz ampoule equipped with the small quartz ampoule of mixed material, carries out secondary vacuum pumping processing by processing and encapsulation process
With secondary seal processing, gained is placed in dual temperature area vertical tube furnace equipped with the big quartz ampoule of small quartz ampoule then, is closed
At reaction.In the present invention, the step of secondary vacuum pumping carried out to the big quartz ampoule is handled and secondary seal handles is preferred
The step of with the vacuumize process and encapsulation process carried out to the small quartz ampoule, is identical, and details are not described herein.
Fig. 1 is the structural schematic diagram of dual temperature area of the present invention vertical tube furnace, and as seen from the figure, the tip of small quartz ampoule is
Sharp cone distal, raw material are placed in small quartz ampoule, and small quartz ampoule is placed in big quartz ampoule, carry out synthetic reaction.
In the present invention, the tip of the quartz ampoule is preferably placed at the position warm area thermocouple horizontal down 5cm, described
The material upper end horizontal position of quartz ampoule is preferably placed at warm area thermocouple horizontal position.Carry out synthetic reaction it
Before, the present invention preferably first carries out vacuumize process to the vacuum degree of furnace body to dual temperature area vertical tube type furnace body and is lower than 10-1Pa, from
And the adverse effect for avoiding gaseous exchange from generating the spatial stability that temperature range is distributed.
In the present invention, the temperature control program of the upper warm area of dual temperature area vertical tube furnace is preferably first warming up to 1050
DEG C, 600min is kept the temperature, first is then carried out and is cooled to 800 DEG C, then carry out second and be cooled to 25 DEG C.
In the present invention, the heating rate of the upper warm area and lower warm area is preferably 50 DEG C/h~100 DEG C/h, and described first
The rate of temperature fall of cooling is preferably 1 DEG C/h, and the rate of temperature fall of second cooling is preferably 20 DEG C/h.The present invention passes through to cooling
The SnSe thermoelectric material monocrystalline type that the control of rate makes.
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
Purity is all larger than to 99.99% SnBr of Sn, Se block and purity greater than 99%2By the original of Sn, Se and Br
Sub- molar ratio is that the proportion of 1:0.97:0.03 is mixed to get mixed material；
The mixed material is synthesized into N-type SnSe thermoelectric material according to vertical gradient dual temperature area's cooling method.
Vertical gradient dual temperature area's cooling method specifically includes the following steps:
1) said mixture material is put into the small quartz ampoule (diameter 5mm) that front end is sharp cone distal, to equipped with mixture
The small quartz ampoule of material is evacuated to vacuum degree less than 10-2Pa, is filled with argon gas, is then evacuated to vacuum degree less than 10-3Pa is used
Flame seals small quartz ampoule；
2) small quartz ampoule obtained by step 1) is placed in big quartz ampoule of the diameter greater than 5mm, it is right according to the method for step 1)
Big quartz ampoule equipped with small quartz ampoule carries out secondary vacuum processing and encapsulation process；
3) being put into big quartz ampoule obtained by step (3) in dual temperature area vertical tube furnace, makes the material upper end of big quartz ampoule
Horizontal position is located at warm area thermocouple horizontal position, is evacuated to vacuum degree to the dual temperature area vertical tube type furnace body and is lower than
10-1Pa；The temperature control program of dual temperature area vertical tube furnace is arranged: warm area is at the uniform velocity warming up to 1050 with the heating rate of 50 DEG C/h
DEG C, 600min is kept the temperature, then warm area is at the uniform velocity cooled to 800 DEG C with the rate of temperature fall of 1 DEG C/h, finally with the rate of temperature fall of 20 DEG C/h
It is cooled to 25 DEG C；Synthetic reaction is carried out according to the temperature control program, obtains N-type SnSe thermoelectric material.
Using in the face of the crystal of the thermoelectric material of the above-mentioned acquisition of Laue X-ray diffraction analysis and out-of-plane orientation, then make
Crystal is cut perpendicular to dissociation face direction with cutting machine.Fig. 2 is the cutting side of N-type SnSe thermoelectric material in embodiment 1
To schematic diagram, Fig. 3 is that the crystal of N-type SnSe thermoelectric material in embodiment 1 dissociates the Laue diffraction pattern spectrum in face, Laue diffraction pattern spectrum
Diffraction spot illustrate resulting materials be SnSe crystal.
Using Seebeck and resistivity test system and laser conductometer to the samples vertical after cutting in dissociation face direction
It is tested, including conductivity, Seebeck coefficient, thermal conductivity etc., obtains the ZT value of the N-type SnSe crystal prototype of Br doping,
Shown in result figure 4.
Embodiment 2~5
The atomic molar of Sn, Se and Br are than being respectively 1:0.975:0.025,1:0.98:0.02,1 in embodiment 2~5:
0.985:0.015 and 1:0.99:0.01, the condition in remaining step embodiment 1 are identical.Table 1 is the current-carrying in Examples 1 to 5
Sub- concentration and most high zt.
Carrier concentration and most high zt in 1 Examples 1 to 5 of table
The atomic molar ratio of Sn, Se and Br are 1:0.97~0.99:0.01~0.03 in mixed material as shown in Table 1, i.e.,
Br Component molar percentage variation range is 1%~3%, and material carrier fluctuation of concentration range is 8.3E18~1.21E19cm-3, and be electronics, illustrate that the material of preparation is N-type semiconductor material.The fluctuation of carrier directly affects final performance figure of merit ZT
Value, the variation range of ZT value are 2.5~2.8, and changing value 0.3, the ZT value of all embodiments is much higher than the foreign side of this patent
The thermoelectric figure of merit of the N-type thermoelectric material of method preparation (ZT is lower than 2.0).
Samples vertical after being cut using Seebeck and resistivity test system and laser conductometer to Examples 1 to 5 in
Dissociation face direction is tested, including conductivity, Seebeck coefficient, thermal conductivity etc., obtains the N-type SnSe crystal prototype of Br doping
ZT value, shown in result figure 4.The use temperature of material is room temperature to 500 DEG C (773K), and most high zt is 500 DEG C (773K)
At a temperature of test obtain.
σ is conductivity in Fig. 4, and S is Seebeck coefficient, and PF is power factor, and κ tot is total thermal conductivity, and κ lat is lattice heat
Conductance, ZT are the thermoelectricity capability figures of merit.Conversion efficiency of thermoelectric is mainly determined by the performance figure of merit ZT of thermoelectric material, by ZT=(S2σ/
κ) T is as it can be seen that at certain temperature T, and material should have big thermoelectromotive force S, and in favor of generating high voltage, (temperature difference is electronic
Gesture also known as Seebeck coefficient), high conductivityσ is in favor of the internal joule energy consumption of reduction, power factor PF=S2σ concentrated expression
The synthesis overall performance electrical performance of material；Total thermal conductivity κ and lattice thermal conductivity κlatThe synthesis heat conveyance performance of material is reflected, it is low
Thermal conductivity κ and lattice thermal conductivity κlatBe conducive to maintain the big temperature difference.However between these thermoelectricity capability parameters mutually according to
Rely, is shifting.The key scientific problems in thermoelectricity field be how the thermoelectricity parameter of coordinated regulation sophisticated interaction, to improve heat
Electric figure of merit ZT, if average ZT value is increased to 2.0 or more from 1.0 applied at present, transfer efficiency can be increased to 20% from 10%.
The application improves conductivityσ's temperature compared with polycrystalline SnS e prepared by melt-synthesizing and high-energy ball milling method
Poor electromotive force S and power factor PF, reduces thermal conductivity κ and lattice thermal conductivity κlat, finally improve ZT value.Most high zt
The 1.0 of the polycrystalline SnS e prepared from melt-synthesizing and high-energy ball milling method are promoted to 2.8.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of N-type SnSe thermoelectric material, which is characterized in that the N-type SnSe thermoelectric material is made of Sn, Se and Br atom,
The atomic molar ratio of described Sn, Se and Br are 1:0.97~0.99:0.01~0.03；The N-type SnSe thermoelectric material is monocrystalline,
The cell parameter abc of the crystal is respectivelyShaft angle α, β, γ are equal
It is 90 °；The ZT value of the N-type SnSe thermoelectric material is 2.0~2.8.
2. SnSe thermoelectric material according to claim 1, which is characterized in that the atomic molar ratio of described Sn, Se and Br is
1:0.98:0.02.
3. the preparation method of N-type SnSe thermoelectric material described in claim 1, comprising the following steps:
1) by Sn, Se and SnBr2It is mixed to get mixed material, the atomic molar ratio of Sn, Se and Br are 1 in the mixed material:
0.97~0.99:0.01~0.03；The mixed material is put into quartz ampoule, vacuumize process is carried out；
2) gained in the step 1) is placed in dual temperature area vertical tube furnace equipped with the quartz ampoule of mixed material, synthesize anti-
It answers, obtains N-type SnSe thermoelectric material；
The temperature control program of the upper warm area of dual temperature area vertical tube furnace in the step 2) are as follows: be first warming up to 1050 DEG C, heat preservation
Then 600min carries out first and is cooled to 800 DEG C, then carries out second and be cooled to 25 DEG C；
The heating rate of the warm area independently is 50 DEG C/h~100 DEG C/h, and the rate of temperature fall of first cooling is 1 DEG C/h,
The rate of temperature fall of second cooling is 20 DEG C/h.
4. preparation method according to claim 3, which is characterized in that the quality purity of the Sn and Se is independently greater than
99.99%, the SnBr2Quality purity be greater than 99%.
5. preparation method according to claim 3, which is characterized in that the vacuum degree in the step 1) after vacuumize process
Less than 10-3Pa。
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