CN108550689A - A kind of preparation method of N-type bismuth telluride-base thermoelectric material - Google Patents
A kind of preparation method of N-type bismuth telluride-base thermoelectric material Download PDFInfo
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- CN108550689A CN108550689A CN201810517151.2A CN201810517151A CN108550689A CN 108550689 A CN108550689 A CN 108550689A CN 201810517151 A CN201810517151 A CN 201810517151A CN 108550689 A CN108550689 A CN 108550689A
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- H—ELECTRICITY
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- H10N15/00—Thermoelectric devices without a junction of dissimilar materials; Thermomagnetic devices, e.g. using the Nernst-Ettingshausen effect
- H10N15/10—Thermoelectric devices using thermal change of the dielectric constant, e.g. working above and below the Curie point
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Abstract
The invention discloses a kind of preparation methods of N-type bismuth telluride-base thermoelectric material, corresponding raw material is weighed with the stoichiometric ratio of N-type bismuth telluride-base crystalline material first and is positioned over Vacuum Package in quartz ampoule, and melting is waved at high temperature, prepare N-type bismuth telluride-base crystalline material using zone-melting process；Using N-type bismuth telluride-base crystalline material as reactive matrix, with I2Reactive matrix and Insertion compound are respectively placed in the both ends of quartz ampoule by molecule as Insertion compound；The region of reactive matrix and Insertion compound will be placed with while being warming up to certain temperature and keeping the temperature, realizes the I under high-temperature steam2Molecular Adsorption；Room temperature is down in two regions respectively by the way of subregion cooling again, obtains I2The N-type bismuth telluride-base thermoelectric material of molecule insertion.This method not only ensure that the orientation and electric property of N-type bismuth telluride, but also reduce lattice thermal conductivity, to realize the raising of N-type bismuth telluride-base thermoelectric material electricity, the coordinated regulation of thermotransport performance and ZT values.
Description
Technical field
The present invention relates to field of thermoelectric material technique more particularly to a kind of preparation methods of N-type bismuth telluride-base thermoelectric material.
Background technology
Thermoelectric material is that the Seebeck effect based on semiconductor and paltie effect realize direct phase between thermal energy and electric energy
A kind of functional material of mutual coupling, due to itself have pollution-free, noiseless, size is small, long lifespan, accurately control etc. it is excellent
Point, thermoelectric material have broad application prospects in thermo-electric generation and two aspect of semiconductor refrigerating.It is high to weigh pyroelectric material performance
Low major parameter is known as thermoelectric figure of merit, ZT=α2σ T/ κ, wherein α is Seebeck coefficient, σ is conductivity, κ is thermal conductivity (packet
Include lattice thermal conductivity κLWith electron thermal conductivity κe), T be absolute temperature.ZT values are bigger, and the conversion efficiency of thermoelectric of material is higher.
Bi2Te3Based alloy is the best thermoelectric material of near room temperature performance, and prepared by commercial bismuth telluride generally use zone melting method, ZT
Value is 1.0 or so, but it is mostly p-type bismuth telluride that ZT values are higher at present, and the ZT values of N-type bismuth telluride material are relatively lower,
This is mainly due to N-type bismuth telluride is more sensitive to the orientation of material and rely on, and in practical applications, high conversion efficiency
Thermo-electric device needs p-type and n type material while having high zt, therefore improves N-type Bi2Te3Thermoelectricity capability for bismuth telluride-base
The application of thermoelectric material is very crucial.
N-type Bi is improved in the prior art2Te3The main method of thermoelectricity capability is to optimize its electric property, but this by doping
Kind method keeps the raising of material ZT values very limited；And N-type Bi is improved using the methods of nanosizing2Te3Thermoelectricity capability can destroy again
Its orientation texture is unfavorable for the collaboration optimization of electricity, hot property.
Invention content
The object of the present invention is to provide a kind of preparation method of N-type bismuth telluride-base thermoelectric material, this method both ensure that N-type
The orientation and electric property of bismuth telluride, and reduce lattice thermal conductivity, to realize N-type bismuth telluride-base thermoelectric material electricity,
The raising of the coordinated regulation and ZT values of thermotransport performance.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of preparation method of N-type bismuth telluride-base thermoelectric material, the method includes：
Step 1 is positioned in quartz ampoule very with the corresponding raw material of stoichiometric ratio weighing of N-type bismuth telluride-base crystalline material
Sky encapsulation, and melting is waved at high temperature, prepare N-type bismuth telluride-base crystalline material using zone-melting process；
Step 2, using prepared N-type bismuth telluride-base crystalline material as reactive matrix, with I2Molecule is as insertion chemical combination
Reactive matrix and Insertion compound are respectively placed in the both ends of quartz ampoule by object；
Step 3, again the quartz ampoule in step 2 vacuumize be placed horizontally at after encapsulation process can subregion temperature control pipe
In formula stove, the region of reactive matrix and Insertion compound will be placed with while being warming up to certain temperature and keeping the temperature, realizes that high temperature steams
I under vapour2Molecular Adsorption；
Step 4 by the way of subregion cooling is dropped in two regions for being placed with reactive matrix and Insertion compound respectively again
To room temperature, I is obtained2The N-type bismuth telluride-base thermoelectric material of molecule insertion.
In step 1, the N-type bismuth telluride-base crystalline material is using Bi, Sb, Te and Se element as material combination.
In step 1, parameter used by the zone-melting process includes：
700~800 DEG C of melting temperature；25 DEG C/min of heating rate；Melting zone 30~40mm of width；Temperature gradient 25~50
℃/cm；25~30mm/h of the speed of growth.
Holding temperature in step 3 is 55 DEG C~113 DEG C, is in I2Sublimation temperature and fusing point between.
In step 4, the mode of the subregion cooling is specially：
The regional temperature for being placed with Insertion compound is reduced with the rate of temperature fall of setting first, it is to be placed to have Insertion compound
Regional temperature reduce by 30 DEG C after, then reduced with same rate of temperature fall and be placed with the regional temperature of reactive matrix, until twoth area
The temperature in domain is down to room temperature.
Set rate of temperature fall is 3-5 DEG C/min, and entire temperature-fall period is always ensured that and is placed with reactive matrix and inserts
Entering two regions of compound, there are positive 30 DEG C of the temperature difference.
As seen from the above technical solution provided by the invention, on the one hand the above method ensure that using crystal orientation
On the other hand the electric property of N-type bismuth telluride utilizes the heterogeneous I being inserted into2Molecular scattering phonon reduces lattice thermal conductivity, from
And realize the raising of N-type bismuth telluride-base thermoelectric material electricity, the coordinated regulation of thermotransport performance and ZT values.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill in field, without creative efforts, other are can also be obtained according to these attached drawings
Attached drawing.
Fig. 1 provides the preparation method flow diagram of N-type bismuth telluride-base thermoelectric material for the embodiment of the present invention；
Fig. 2 is provided the schematic diagram of reaction process by the embodiment of the present invention；
Fig. 3 is I described in the embodiment of the present invention2N-type Bi before and after intercalation2Te2.7Se0.3Lattice thermal conductivity vary with temperature song
Line schematic diagram；
Fig. 4 is I described in the embodiment of the present invention2N-type Bi before and after intercalation2Te2.7Se0.3Thermoelectric figure of merit ZT vary with temperature and show
It is intended to.
Specific implementation mode
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, belongs to protection scope of the present invention.
The embodiment of the present invention is described in further detail below in conjunction with attached drawing, is implemented as shown in Figure 1 for the present invention
Example provides the preparation method flow diagram of N-type bismuth telluride-base thermoelectric material, the method includes：
Step 1 is positioned in quartz ampoule very with the corresponding raw material of stoichiometric ratio weighing of N-type bismuth telluride-base crystalline material
Sky encapsulation, and melting is waved at high temperature, prepare N-type bismuth telluride-base crystalline material using zone-melting process；
In the step, the N-type bismuth telluride-base crystalline material is using Bi, Sb, Te and Se element as material combination.
Parameter includes used by the zone-melting process：
700~800 DEG C of melting temperature；25 DEG C/min of heating rate；Melting zone 30~40mm of width；Temperature gradient 25~50
℃/cm；25~30mm/h of the speed of growth.
Step 2, using prepared N-type bismuth telluride-base crystalline material as reactive matrix, with I2Molecule is as insertion chemical combination
Reactive matrix and Insertion compound are respectively placed in the both ends of quartz ampoule by object；
It is illustrated in figure 2 the schematic diagram of the provided reaction process of the embodiment of the present invention, left side is with I in Fig. 22Molecule conduct
The region of Insertion compound, right side are the region using N-type bismuth telluride-base crystalline material as reactive matrix.
Step 3, again the quartz ampoule in step 2 vacuumize be placed horizontally at after encapsulation process can subregion temperature control pipe
In formula stove, the region of reactive matrix and Insertion compound will be placed with while being warming up to certain temperature and keeping the temperature, realizes that high temperature steams
I under vapour2Molecular Adsorption；
Here, holding temperature is 55 DEG C~113 DEG C, is in I2Sublimation temperature and fusing point between, to ensure I2It generates higher
Vapour pressure, the active force of vapour pressure can be by I2The interlayer that molecule is inserted into bismuth telluride forms intercalation compound, as shown in Figure 2
Distil I at high temperature2Molecule, soaking time can be 6-24 hours.
Step 4 by the way of subregion cooling is dropped in two regions for being placed with reactive matrix and Insertion compound respectively again
To room temperature, I is obtained2The N-type bismuth telluride-base thermoelectric material of molecule insertion.
In the step, the mode of subregion cooling is specially：
The regional temperature for being placed with Insertion compound is reduced with the rate of temperature fall of setting first, it is to be placed to have Insertion compound
Regional temperature reduce by 30 DEG C after, then reduced with same rate of temperature fall and be placed with the regional temperature of reactive matrix, until twoth area
The temperature in domain is down to room temperature.
Above-mentioned set rate of temperature fall is 3-5 DEG C/min, and entire temperature-fall period is always ensured that and is placed with reactive matrix
There are positive 30 DEG C of the temperature difference with two regions of Insertion compound, to prevent extra I2Molecule is finally sublimated in bismuth telluride sample
Surface.
Above-mentioned preparation method is described in detail with specific example below：
Example 1, with N-type Bi2Te2.7Se0.3Stoichiometric ratio weigh raw material Bi, Te, Se powder, original powder is placed
10 are evacuated in quartz ampoule-5The processing of Pa post packages, quartz ampoule are placed in rocking furnace at 800 DEG C after melting 4 hours with furnace cooling
But to room temperature；
Quartz ampoule is put into growing by zone melting stove again, condition is melted in setting area：720 DEG C of melting temperature, heating rate
25 DEG C/min, melting zone width 30mm, 25 DEG C/cm of temperature gradient, speed of growth 25mm/h, prepare N-type
Bi2Te2.7Se0.3Crystalline material.
By N-type Bi2Te2.7Se0.3Crystal is as reactive matrix, suitable I2Powder is respectively placed in stone as Insertion compound
The both ends of English pipe, quartz ampoule vacuumize (to 10-5Pa) being placed horizontally at after encapsulation process can be in the tube furnace of subregion temperature control, by tellurium
Change bismuth region and I2Powder region is warming up to 60 DEG C and keeps the temperature 10 hours simultaneously.
Then, I is first reduced with the rate of temperature fall of 5 DEG C/min2The temperature in powder region, waits for I2After powder regional temperature reduces by 30 DEG C,
Bi is reduced with same 5 DEG C/min rate of temperature fall again2Te2.7Se0.3Regional temperature, until the temperature in two regions is down to room temperature,
It is final to obtain I2The N-type Bi of molecule insertion2Te2.7Se0.3Intercalation thermoelectric material.
Further characterization measures above-mentioned N-type Bi2Te2.7Se0.3Carry out I2Related thermoelectricity capability before and after intercalation simultaneously compares, and obtains
To I shown in Fig. 32N-type Bi before and after intercalation2Te2.7Se0.3Lattice thermal conductivity vary with temperature shown in curve synoptic diagram and Fig. 4
I2N-type Bi before and after intercalation2Te2.7Se0.3Thermoelectric figure of merit ZT vary with temperature schematic diagram.
As can be seen from Figure 3：Due to the I of insertion2Molecule has stronger scattering effect, I to phonon2N-type after intercalation
Bi2Te2.7Se0.3Lattice thermal conductivity be below I in entire Range of measuring temp2Bi before intercalation2Te2.7Se0.3Lattice thermal conductivity
Rate；As can be seen from Figure 4：I2N-type Bi after intercalation2Te2.7Se0.3ZT values in entire Range of measuring temp be higher than I2Before intercalation
Bi2Te2.7Se0.3ZT values.
The above results illustrate the I prepared by vapor adsorption process in the present embodiment2Intercalation N-type Bi2Te2.7Se0.3Pyroelectricity
It can be optimized.
Example 2, with N-type Bi2Te2.7Se0.3Stoichiometric ratio weigh raw material Bi, Te, Se powder, original powder is placed
10 are evacuated in quartz ampoule-5The processing of Pa post packages, quartz ampoule are placed in rocking furnace at 800 DEG C after melting 4 hours with furnace cooling
But to room temperature；Quartz ampoule is put into growing by zone melting stove again, condition is melted in setting area：720 DEG C of melting temperature, 25 DEG C of heating rate/
Min, melting zone width 30mm, 25 DEG C/cm of temperature gradient, speed of growth 25mm/h, prepare N-type Bi2Te2.7Se0.3Crystalline material.
By N-type Bi2Te2.7Se0.3Crystal is as reactive matrix, suitable I2Powder is respectively placed in the two of quartz ampoule as Insertion compound
End, quartz ampoule vacuumize (to 10-5Pa) being placed horizontally at after encapsulation process can be in the tube furnace of subregion temperature control, by bismuth telluride region
With I2Powder region is warming up to 60 DEG C and keeps the temperature 20 hours simultaneously.Then, I is first reduced with the rate of temperature fall of 5 DEG C/min2The temperature in powder region
Degree, waits for I2After powder regional temperature reduces by 30 DEG C, then with same 5 DEG C/min rate of temperature fall reduction Bi2Te2.7Se0.3Region temperature
Degree finally obtains I until the temperature in two regions is down to room temperature2The N-type Bi of molecule insertion2Te2.7Se0.3Intercalation thermoelectric material.
Characterization measures above-mentioned N-type Bi2Te2.7Se0.3Carry out I2Related thermoelectricity capability before and after intercalation simultaneously compares, and obtains similar
In Fig. 3, Fig. 4 as a result, showing the I prepared in the present embodiment2Intercalation N-type Bi2Te2.7Se0.3Thermoelectricity capability optimized.
Example 3, with N-type Bi2Te2.7Se0.3Stoichiometric ratio weigh raw material Bi, Te, Se powder, original powder is placed
10 are evacuated in quartz ampoule-5The processing of Pa post packages, quartz ampoule are placed in rocking furnace at 800 DEG C after melting 4 hours with furnace cooling
But to room temperature；Quartz ampoule is put into growing by zone melting stove again, condition is melted in setting area：720 DEG C of melting temperature, 25 DEG C of heating rate/
Min, melting zone width 30mm, 25 DEG C/cm of temperature gradient, speed of growth 25mm/h, prepare N-type Bi2Te2.7Se0.3Crystalline material.
By N-type Bi2Te2.7Se0.3Crystal is as reactive matrix, suitable I2Powder is respectively placed in the two of quartz ampoule as Insertion compound
End, quartz ampoule vacuumize (to 10-5Pa) being placed horizontally at after encapsulation process can be in the tube furnace of subregion temperature control, by bismuth telluride region
With I2Powder region is warming up to 80 DEG C and keeps the temperature 10 hours simultaneously.Then, I is first reduced with the rate of temperature fall of 5 DEG C/min2The temperature in powder region
Degree, waits for I2After powder regional temperature reduces by 30 DEG C, then with same 5 DEG C/min rate of temperature fall reduction Bi2Te2.7Se0.3Region temperature
Degree finally obtains I until the temperature in two regions is down to room temperature2The N-type Bi of molecule insertion2Te2.7Se0.3Intercalation thermoelectric material.
Characterization measures above-mentioned N-type Bi2Te2.7Se0.3Carry out I2Related thermoelectricity capability before and after intercalation simultaneously compares, and obtains similar
In Fig. 3, Fig. 4 as a result, showing the I prepared in the present embodiment2Intercalation N-type Bi2Te2.7Se0.3Thermoelectricity capability optimized.
Example 4, with N-type Bi2Te2.7Se0.3Stoichiometric ratio weigh raw material Bi, Te, Se powder, original powder is placed
10 are evacuated in quartz ampoule-5The processing of Pa post packages, quartz ampoule are placed in rocking furnace at 800 DEG C after melting 4 hours with furnace cooling
But to room temperature；Quartz ampoule is put into growing by zone melting stove again, condition is melted in setting area：720 DEG C of melting temperature, 25 DEG C of heating rate/
Min, melting zone width 30mm, 25 DEG C/cm of temperature gradient, speed of growth 25mm/h, prepare N-type Bi2Te2.7Se0.3Crystalline material.
By N-type Bi2Te2.7Se0.3Crystal is as reactive matrix, suitable I2Powder is respectively placed in the two of quartz ampoule as Insertion compound
End, quartz ampoule vacuumize (to 10-5Pa) being placed horizontally at after encapsulation process can be in the tube furnace of subregion temperature control, by bismuth telluride region
With I2Powder region is warming up to 100 DEG C and keeps the temperature 10 hours simultaneously.Then, I is first reduced with the rate of temperature fall of 3 DEG C/min2The temperature in powder region
Degree, waits for I2After powder regional temperature reduces by 30 DEG C, then with same 3 DEG C/min rate of temperature fall reduction Bi2Te2.7Se0.3Region temperature
Degree finally obtains I until the temperature in two regions is down to room temperature2The N-type Bi of molecule insertion2Te2.7Se0.3Intercalation thermoelectric material.
Characterization measures above-mentioned N-type Bi2Te2.7Se0.3Carry out I2Related thermoelectricity capability before and after intercalation simultaneously compares, and obtains similar
In Fig. 3, Fig. 4 as a result, showing the I prepared in the present embodiment2Intercalation N-type Bi2Te2.7Se0.3Thermoelectricity capability optimized.
Example 5, with N-type Bi2Te2.5Se0..5Stoichiometric ratio weigh raw material Bi, Te, Se powder, original powder is placed
10 are evacuated in quartz ampoule-5The processing of Pa post packages, quartz ampoule are placed in rocking furnace at 800 DEG C after melting 4 hours with furnace cooling
But to room temperature；Quartz ampoule is put into growing by zone melting stove again, condition is melted in setting area：720 DEG C of melting temperature, 25 DEG C of heating rate/
Min, melting zone width 30mm, 25 DEG C/cm of temperature gradient, speed of growth 25mm/h, prepare N-type Bi2Te2.5Se0..5Crystalline material.
By N-type Bi2Te2.5Se0..5Crystal is as reactive matrix, suitable I2Powder is respectively placed in the two of quartz ampoule as Insertion compound
End, quartz ampoule vacuumize (to 10-5Pa) being placed horizontally at after encapsulation process can be in the tube furnace of subregion temperature control, by bismuth telluride region
With I2Powder region is warming up to 100 DEG C and keeps the temperature 10 hours simultaneously.Then, I is first reduced with the rate of temperature fall of 3 DEG C/min2The temperature in powder region
Degree, waits for I2After powder regional temperature reduces by 30 DEG C, then with same 3 DEG C/min rate of temperature fall reduction Bi2Te2.5Se0..5Region temperature
Degree finally obtains I until the temperature in two regions is down to room temperature2The N-type Bi of molecule insertion2Te2.5Se0..5Intercalation thermoelectric material.
Characterization measures above-mentioned N-type Bi2Te2.5Se0..5Carry out I2Related thermoelectricity capability before and after intercalation simultaneously compares, and obtains similar
In Fig. 3, Fig. 4 as a result, showing the I prepared in the present embodiment2Intercalation N-type Bi2Te2.5Se0..5Thermoelectricity capability optimized.
It is worth noting that, the content not being described in detail in the embodiment of the present invention belongs to professional and technical personnel in the field's public affairs
The prior art known.
In conclusion the preparation method that the embodiment of the present invention is provided both ensure that the orientation and electricity of N-type bismuth telluride
Performance, and utilize the heterogeneous I being inserted into2Molecular scattering phonon reduces lattice thermal conductivity, to realize N-type bismuth telluride-based thermoelectric
The raising of material electricity, the coordinated regulation of thermotransport performance and ZT values.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (6)
1. a kind of preparation method of N-type bismuth telluride-base thermoelectric material, which is characterized in that the method includes：
Step 1 is positioned over vacuum seal in quartz ampoule with the corresponding raw material of stoichiometric ratio weighing of N-type bismuth telluride-base crystalline material
Dress, and melting is waved at high temperature, prepare N-type bismuth telluride-base crystalline material using zone-melting process；
Step 2, using prepared N-type bismuth telluride-base crystalline material as reactive matrix, with I2Molecule, will as Insertion compound
Reactive matrix and Insertion compound are respectively placed in the both ends of quartz ampoule；
Step 3, again the quartz ampoule in step 2 vacuumize be placed horizontally at after encapsulation process can subregion temperature control tube furnace
It is interior, the region of reactive matrix and Insertion compound will be placed with while being warming up to certain temperature and keeping the temperature, realized under high-temperature steam
I2Molecular Adsorption；
Room by the way of subregion cooling is down in two regions for being placed with reactive matrix and Insertion compound by step 4 respectively again
Temperature obtains I2The N-type bismuth telluride-base thermoelectric material of molecule insertion.
2. the preparation method of N-type bismuth telluride-base thermoelectric material according to claim 1, which is characterized in that in step 1, institute
N-type bismuth telluride-base crystalline material is stated using Bi, Sb, Te and Se element as material combination.
3. the preparation method of N-type bismuth telluride-base thermoelectric material according to claim 1, which is characterized in that in step 1, institute
Stating parameter used by zone-melting process includes：
700~800 DEG C of melting temperature；25 DEG C/min of heating rate；Melting zone 30~40mm of width；25~50 DEG C/cm of temperature gradient；
25~30mm/h of the speed of growth.
4. the preparation method of N-type bismuth telluride-base thermoelectric material according to claim 1, which is characterized in that guarantor in step 3
Temperature is 55 DEG C~113 DEG C, is in I2Sublimation temperature and fusing point between.
5. the preparation method of N-type bismuth telluride-base thermoelectric material according to claim 1, which is characterized in that in step 4, institute
Stating the mode that subregion cools down is specially：
The regional temperature for being placed with Insertion compound, the area to be placed for having Insertion compound are reduced with the rate of temperature fall of setting first
After domain temperature reduces by 30 DEG C, then the regional temperature for being placed with reactive matrix is reduced with same rate of temperature fall, until two regions
Temperature is down to room temperature.
6. the preparation method of N-type bismuth telluride-base thermoelectric material according to claim 5, which is characterized in that set cooling
Rate is 3-5 DEG C/min, and entire temperature-fall period is always ensured that two regions for being placed with reactive matrix and Insertion compound exist
Positive 30 DEG C of the temperature difference.
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| CN110098313A (en) * | 2019-04-22 | 2019-08-06 | 武汉科技大学 | A kind of preparation method of preferred orientation p-type bismuth telluride-base polycrystalline bulk thermoelectric material |
| CN117166039A (en) * | 2023-08-03 | 2023-12-05 | 武汉理工大学 | Preparation method of bismuth telluride-based thermoelectric material capable of synchronously improving mechanical property and thermoelectric property |
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