CN108198934A - A kind of composite thermoelectric material and preparation method thereof - Google Patents
A kind of composite thermoelectric material and preparation method thereof Download PDFInfo
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- CN108198934A CN108198934A CN201711461912.9A CN201711461912A CN108198934A CN 108198934 A CN108198934 A CN 108198934A CN 201711461912 A CN201711461912 A CN 201711461912A CN 108198934 A CN108198934 A CN 108198934A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/01—Manufacture or treatment
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/853—Thermoelectric active materials comprising inorganic compositions comprising arsenic, antimony or bismuth
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/855—Thermoelectric active materials comprising inorganic compositions comprising compounds containing boron, carbon, oxygen or nitrogen
Abstract
The present invention provides a kind of composite thermoelectric materials and preparation method thereof, belong to field of thermoelectric material technique, the composite thermoelectric material includes Cu, La, Se, N and adulterates SiC, wherein N doping SiC grain sizes are respectively less than 100nm, the ratio that the content of N doping SiC is 0.1 1 mass %, Cu and Se is 1.5 1.9:1.The thermoelectricity capability of composite thermoelectric material prepared by the present invention, mechanical property are greatly improved.
Description
Technical field
The invention belongs to field of thermoelectric material technique, and in particular to a kind of nano composite thermoelectric materials and preparation method thereof.
Background technology
Compound semiconductor is by the element of at least two types rather than a type of element (such as silicon or germanium) structure
Into and as semiconductor compound.It has been developed for various types of compound semiconductors and these compounds is partly led
Body is used for various industrial circles at present.In general, compound semiconductor can be used for utilizing Peltier effect (Peltier
Effect thermoelectric conversion element), the light-emitting device (such as light emitting diode or laser diode) using opto-electronic conversion effect
With fuel cell etc..
Particularly, thermoelectric conversion element for heat to electricity conversion generate electricity or heat to electricity conversion cooling application, and generally include with
The mode of series connection is electrically connected and hot linked N-type thermoelectric semiconductor and p-type thermoelectric semiconductor in parallel.Heat to electricity conversion
Power generation is thermal energy to be made to be converted into electric energy by using the thermo-electromotive force by means of generating the temperature difference in thermoelectric conversion element and generating
And the method to generate electricity.In addition, heat to electricity conversion cooling be by using during the both ends that thermoelectric conversion element is flowed through when DC current
The method that the effect of the temperature difference makes electric energy be converted into thermal energy and generates cooling is generated between thermoelectric conversion element both ends.Heat to electricity conversion member
The conversion efficiency of thermoelectric of part is generally dependent on the performance index value or ZT of thermo-electric converting material.Here, ZT (thermoelectric figure of merit) can be with
It is determined according to Seebeck coefficient (Seebeck coefficient), conductivity and thermal conductivity, and as ZT values increase, heat
The performance of electric transition material is more preferable.It has proposed now and has developed many thermoelectric materials that can be used for thermoelectric conversion element, and
And therein it is proposed that CuxSe (x≤2) as Cu-Se base thermoelectricity materials and developed into this material.
Particularly, be recently reported realizes relatively low thermal conductivity and high thermoelectric figure of merit in CuxSe (1.98≤x≤2).
However, observing fairly good thermoelectric figure of merit at 600 DEG C to 727 DEG C, but find hot at a temperature of less than or equal to 600 DEG C
The electric figure of merit is very low, averagely less than 1.3.Although thermoelectric material has high thermoelectric figure of merit at high temperature, if the thermoelectricity material
Material has low thermoelectric figure of merit at low temperature, then such thermoelectric material is not preferred, and particularly, is unsuitable for for power generation
Thermoelectric material.Even if such thermoelectric material is applied to high temperature heat source, some region of the material is also due to the material sheet
The temperature gradient of body and be subjected to the temperature more much lower than desired temperature.Therefore, it is necessary to develop following thermoelectric material：The thermoelectricity material
Material still has in the temperature range less than 600 DEG C (such as 100 DEG C to 600 DEG C)>1.6 high thermoelectric figure of merit.
Invention content
For above-mentioned technical problem, the present invention provides a kind of composite thermoelectric material, the composite thermoelectric material include Cu,
La, Se, N adulterate SiC, and wherein N doping SiC grain sizes are respectively less than 100nm, and the content of N doping SiC is 0.1-1 mass %, Cu and Se
Ratio be 1.5-1.9:1, La content is 1-5 mass %.
Further, the ratio of wherein Cu and Se is 1.8:1.
Further, wherein, the content that N is adulterated in SiC is 0.5 mass %.
Further, wherein, the grain size of N doping SiC is 50nm.
Further, wherein, the content of the La is 2%.
The present invention also provides the method for preparing above-mentioned composite thermoelectric material, wherein, the method includes
1) N doping SiC powders are carried out below ball milling mixing to grain size 100nm；
2) in proportion using Cu powder, La powder, Se powder as raw material, grinding carries out melting after forming particle under vacuum sealing environment
Afterwards, the powder made from step 1 is added in, is stirred evenly, is cooled down；
3) solid solution made from step 2 is pulverized, and the powder of grinding is fitted into graphite jig, and mold is placed in electric discharge
Sintering obtains product in plasma agglomeration furnace cavity.
Further, wherein, the sintering condition of discharge plasma sintering furnace cavity is in step 4：Apply the axis of 30-2GPa
It to pressure, is sintered under vacuum condition, is heated up with the heating rate of 100-150 DEG C/min, sintering temperature is 800~900 DEG C, heat preservation
10~20min cools to room temperature with the furnace.
According to method provided by the invention, wherein, the ball milling mixing described in step (1) at 7500-10000 revs/min,
For example, it is carried out 3-5 hours under 8000 revs/min of rotating speed.
The present invention prepares in composite thermoelectric material matrix that there are the nano composite structures of amorphous/nanocrystalline, crystal grain to be shown
Write refinement.Using the SiC for adulterating N element, nano particle is formed in nanocrystalline melting process in metal and is formed as amorphous state
Composite construction, Cu are located at the grain boundary of amorphous/nanocrystalline, which reduces heat to electricity conversion energy barrier, while N is adulterated
SiC can effectively improve thermoelectricity capability and electric conductivity.A certain proportion of La elements are added, which adds
Add, due to its special electronic structure, can further Microalloying Effect and La is easily in grain boundaries segregation, enhance crystalline substance
Thermoelectricity capability so as to further reduce heat to electricity conversion energy barrier and lattice thermal energy, improves in boundary.The thermoelectric material of the present invention can be
There is low thermal diffusivity (thermal diffusivity), lower thermal conductivity, height in wide temperature range between 100 DEG C to 600 DEG C
Seebeck coefficient and high thermoelectric figure of merit.
In the present invention, to the Particle size requirements of SiC powder in 100nm hereinafter, smaller grain size is conducive to the equal of thermoelectric material
Even mixing, and lattice thermal conductivity is advantageously reduced, grain size is the smaller the better, it is contemplated that the balance of cost problem and performance, preferably
50nm。
It has also been found that, the product being prepared can be effectively improved by adding a certain proportion of N doping SiC and La simultaneously
Mechanical property, La elements have refining alloy tissue, reduce intergranular away from effect, while its can with impurity element P etc. into
Row reaction, can make alloy graining temperature range narrow so as to improve the casting character of alloy, and can mitigate cracking and raising
Compactness, and the N of nanometer phase adulterates its facilitation effect with collaboration of SiC.
Compared with prior art, the invention has the advantages that：
(1) SiC is adulterated by adding a certain proportion of La and N, the mechanical property for the thermoelectric material being prepared also obtains
A degree of raising；
(2) amorphous of the nano composite structure/crystalline state thermoelectric material prepared by the present invention, the thermoelectricity capability of material, especially
It is that low temperature thermoelectricity capability is greatly improved.
Specific embodiment
The present invention provides a kind of composite thermoelectric material, the composite thermoelectric material includes Cu, La, Se, N and adulterates SiC,
Middle N doping SiC grain sizes are respectively less than 100nm, and the content that N adulterates SiC is that the ratio of 0.1-1 mass %, Cu and Se are 1.5-1.9:
1, La content is 1-5 mass %.
Embodiment 1-5 and comparative example 1-8 are prepared as follows according to the formula of table 1
1) SiC is weighed in the glove box enclosed by the formula of table 1 in Ar atmosphere, is placed in interval ball milling in the ball grinder of steel
3 hours, the wherein rotating speed of ball grinder was 8000 revs/min.
2) using high-frequency induction smelting in suspension equipment, with Cu blocks (purity 99.99%), La blocks (purity 99.999%), Se
Block (purity 99.99%) is raw material, and being formulated proportioning in an ar atmosphere according to table 1 weighs, and prepared raw material is put into red copper earthenware
Melting is carried out in crucible, the powder of step 1 is added in after melting, is stirred evenly, using guarantor of the argon gas as fusion process after deoxidation
Protect atmosphere, peak power 14kw.
3) using induction melting fast quenching furnace apparatus, the ingot casting of step 2 is packed into the quartz ampoule of lower ending opening, then vertically
It is placed in the induction melting coil of fast quenching equipment cavity, cavity vacuumizes, and being filled with protection argon gas to cavity by fast quenching equipment reaches
To -0.03MPa, adjusting injection pressure is 0.02MPa, induction melting block is made to reach molten state, melt is being sprayed onto 40m/s turns
It is thrown away on the copper roller of speed, into band, collects band.
4) band of collection is placed in the glove box of argon gas atmosphere of the oxygen content less than 0.5ppm and pulverized, will ground
Powder be fitted into graphite jig, mold is placed in SPS sintering cavities, applies the axial compressive force of 30MPa, is less than in total gas pressure
It is sintered under the vacuum condition of 5Pa, is heated up with the heating rate of 100-150 DEG C/min, sintering temperature is 800-900 DEG C, keeps the temperature 10-
20min cools to room temperature with the furnace, obtains the nano composite structure solid solution there are amorphous/nanocrystalline.
The formula of 1 each embodiment of table and comparative example
Performance detection：The thermal conductivity of material is according to the thermal diffusion measured using TC-1200RH type laser pulses thermal analyzer
The density of coefficient, specific heat and material is calculated.The Seebeck coefficient and conductivity of material use ZEM-2 electrical property test instruments 2
It measures.The thermoelectric figure of merit of material presses formula Z=α according to above-mentioned measurement result2σ/κ is obtained.
The plate of 0.1mm thickness suppressed using embodiment and comparative example, in vacuum atmosphere in 400 DEG C of 10mm ×
After being brazed between the potsherd of 10mm × 20mm, the test film of 3mm × 4mm × 40mm is cut out, passes through four-point bending test
Each 10 points of fracture strength is measured according to JIS R1601.(test method is carried out according to JIS R1601).
Comparative example and comparative example 1,2 find that control La elements in suitable content range, help to improve product
Properties, the reduced performance that excessive or too small La will lead to product.Comparative example and comparative example 3,4, it is known that control
The molar ratio of Cu and Se can effectively improve the thermoelectricity capability of product, thus it is speculated that be 1.5-1.9:Cu and Se in the range of 1 is formed
Lattice energy barrier it is lower.Comparative example and comparative example 5,6, find the SiC of a certain range of N dopings, can be effective
The thermoelectricity capability and fracture strength of product are improved, and ensures that conductivity does not decline integrally.Comparative example and comparative example 7,8,
Addition N doping SiC can be effectively improved thermoelectricity capability, it has further been found that the grain size of N doping SiC needs to control in a certain range
It is interior, thermoelectricity capability and fracture strength can be enhanced while conductivity is ensured.To sum up, under the formula of the present invention, various groups
Divide and cooperate, synergistic effect, so as to which the technical performance of the product of the present invention greatly improved.
More than content is it cannot be assumed that present invention specific implementation is confined to these explanations, for the technical field of the invention
Those of ordinary skill for, under the premise of present inventive concept is not departed from, several simple deduction or replace can also be made, all should
When being considered as belonging to present invention scope of patent protection determined by the appended claims.
Claims (7)
1. a kind of composite thermoelectric material, which is characterized in that the composite thermoelectric material includes Cu, La, Se, N and adulterates SiC, wherein N
Doping SiC grain sizes are respectively less than 100nm, and the content that N adulterates SiC is that the ratio of 0.1-1 mass %, Cu and Se are 1.5-1.9:1, La
Content be 1-5 mass %.
2. composite thermoelectric material according to claim 1, which is characterized in that the ratio of Cu and Se is 1.8:1.
3. composite thermoelectric material according to claim 1, which is characterized in that the content that N is adulterated in SiC is 0.5 mass %.
4. composite thermoelectric material according to claim 1, which is characterized in that the grain size of SiC is 50nm.
5. composite thermoelectric material according to claim 1, which is characterized in that the content of the La is 2%.
6. a kind of preparation method according to claim 1-5 any one of them composite thermoelectric materials, which is characterized in that including with
Lower step：
1) N doping SiC powders are carried out below ball milling mixing to grain size 100nm；
2) in proportion using Cu powder, La powder, Se powder as raw material, grinding is formed after particle under vacuum sealing environment carry out melting after,
The powder made from step 1 is added in, is stirred evenly, is cooled down；
3) solid solution is pulverized made from step 2, and the powder of grinding is fitted into graphite jig, and mold is placed in plasma discharging
Sintering obtains product in sintering furnace cavity.
7. the preparation method of composite thermoelectric material according to claim 6, which is characterized in that plasma discharging in step 3
Sintering furnace cavity sintering condition be：Apply the axial compressive force of 30-2GPa, be sintered under vacuum condition, with 100-150 DEG C/min's
Heating rate heats up, and sintering temperature is 800~900 DEG C, keeps the temperature 10~20min, cools to room temperature with the furnace.
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Cited By (2)
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| CN110444656A (en) * | 2019-08-20 | 2019-11-12 | 上海第二工业大学 | A kind of preparation method of cuprous sulfide complex silicon carbide block thermoelectric material |
| CN110592459A (en) * | 2019-09-10 | 2019-12-20 | 大连理工大学 | High-entropy Half-Heusler thermoelectric material with low lattice thermal conductivity and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110444656A (en) * | 2019-08-20 | 2019-11-12 | 上海第二工业大学 | A kind of preparation method of cuprous sulfide complex silicon carbide block thermoelectric material |
| CN110444656B (en) * | 2019-08-20 | 2022-10-04 | 上海第二工业大学 | Preparation method of cuprous sulfide composite silicon carbide block thermoelectric material |
| CN110592459A (en) * | 2019-09-10 | 2019-12-20 | 大连理工大学 | High-entropy Half-Heusler thermoelectric material with low lattice thermal conductivity and preparation method thereof |
| CN110592459B (en) * | 2019-09-10 | 2022-02-08 | 大连理工大学 | High-entropy Half-Heusler thermoelectric material with low lattice thermal conductivity and preparation method thereof |
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