CN107452865A - A kind of gold nano grain cladding nanometer chip architecture Sb2Te3The preparation method of thermoelectric material - Google Patents

A kind of gold nano grain cladding nanometer chip architecture Sb2Te3The preparation method of thermoelectric material Download PDF

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CN107452865A
CN107452865A CN201710487501.0A CN201710487501A CN107452865A CN 107452865 A CN107452865 A CN 107452865A CN 201710487501 A CN201710487501 A CN 201710487501A CN 107452865 A CN107452865 A CN 107452865A
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aqueous solution
thermoelectric material
chip architecture
nanometer chip
configure
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CN107452865B (en
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王自昱
杨帆
雷刚勤
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Dongfeng Commercial Vehicle Co Ltd
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Dongfeng Commercial Vehicle Co Ltd
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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
    • 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
    • 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
    • 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
    • H10N10/852—Thermoelectric active materials comprising inorganic compositions comprising tellurium, selenium or sulfur

Abstract

A kind of gold nano grain cladding nanometer chip architecture Sb2Te3The preparation method of thermoelectric material, including following step：Binary pure phase Sb is made first by solvent-thermal method2Te3Powder washing and drying again；Then 0.01mol/L HAuCl, is configured4The AgNO of the aqueous solution, 0.1%wt3The Na of the aqueous solution, 0.1%wt3C6H5O7The aqueous solution；Then 1ml HAuCl are sequentially added in the aqueous solution of 100ml boilings4、20~40μl AgNO3With 1 ~ 6ml Na3C6H5O7Mixed liquor, and 0.197 gram of Sb2Te3Powder；Finally mixed liquor centrifuge washing is dried, obtains powdered product 1%Au@Sb2Te3.Effectively lifting pure phase nanometer chip architecture Sb2Te3Thermoelectric figure of merit, obtained compound Sb2Te3Thermoelectric material ZT values compared with original structure can lift more than 1 times.

Description

A kind of gold nano grain cladding nanometer chip architecture Sb2Te3The preparation method of thermoelectric material
Technical field
The present invention relates to a kind of material fabrication process, and nanometer sheet is coated more specifically to a kind of gold nano grain Structure Sb2Te3The preparation method of thermoelectric material, belongs to field of material synthesis technology.
Background technology
Thermoelectric material is that the advanced material that heat energy is mutually changed with electric energy is statically realized in a kind of movement by carrier, As people's environmental protection and the raising of awareness of saving energy, the research related to thermoelectric material are also more and more；The thermoelectricity of thermoelectric material turns Change efficiency and depend primarily on figure of merit ZT, the ZT values of thermoelectric material are the higher the better.Sb2Te3Compound is that current use is most ripe One of commercialization thermoelectric material, it is at 200 DEG C to the regional computer thermoelectric material that can be best of room temperature.
Discovered in recent years, nanostructured thermoelectric materials (nanometer sheet, nano dot, nano wire, nanocrystalline) greatly improve ZT The potentiality of value；The wherein nanometer chip architecture Sb of solvent structure2Te3Thermoelectric material is because thermal conductivity declines to a great extent and exists Structural anisotropy, it is the study hotspot in nanostructured thermoelectric materials.But nanometer chip architecture Sb2Te3Thermoelectric material with it is micro- Rice structural material is compared, and extremely low thermal conductivity is shown because nano material crystal boundary increases；And the transport of carrier is simultaneously Receive scattering and suppress, cause power factor the sign deteriorated occur, ZT values only reach 0.35 or so in 500K.
The content of the invention
The present invention is directed to existing nanometer chip architecture Sb2Te3There is deterioration sign, ZT in power factor existing for thermoelectric material Value is 500K only reaches 0.35 or so the problems such as, there is provided a kind of gold nano grain cladding nanometer chip architecture Sb2Te3Thermoelectric material Preparation method.
To achieve the above object, technical solution of the invention is：A kind of gold nano grain coats nanometer chip architecture Sb2Te3The preparation method of thermoelectric material, including following step：
Step 1, binary pure phase Sb is made using solvent-thermal method2Te3Powder, it is then centrifuged for washing and drying, and ESEM Its pattern is observed, confirms as a nanometer chip architecture；
Step 2, configure 0.01mol/L HAuCl4The aqueous solution；
Step 3, configure 0.1%wt AgNO3The aqueous solution；
Step 4, configure 0.1%wt Na3C6H5O7The aqueous solution；
Step 5, in the aqueous solution of 100ml boilings, sequentially add 1ml HAuCl4, 20~40 μ lAgNO3With 1~6ml Na3C6H5O7Mixed liquor, and 0.197 gram of Sb2Te3Powder, and stir；
Step 6, the mixed liquor in step 5 reacts under fluidized state to be stopped heating after 15min and carries out natural cooling, Keep persistently stirring reaction solution 2 hours in cooling procedure, last centrifuge washing drying, so as to obtain powdered product 1%Au@ Sb2Te3。
Compared with prior art, the beneficial effects of the invention are as follows：
1st, composition of raw materials is concise, and technological process is simple and easy to control；Tested by product property homogeneity, compare 5 synthesis The product thermoelectricity capability of batch, ZT values deviation is within 5%, therefore products therefrom consistency of performance is high.
2nd, 1%Au@Sb provided by the invention2Te3Concentration be an optimal Au addition concentration, under 1%Au concentration, energy Appropriate extra electron is enough provided, compensate for the negative effect that energy filtering effect reduces electron mobility；Further pass through Verification experimental verification, under the concentration, material electric conductivity increases on the contrary to a certain extent, and other Au concentration (use same procedure Synthesize 0.5%Au, 2%Au, 3%Au, 4%Au) it can reduce electrical conductivity.
Brief description of the drawings
Sb synthesized when being 1%Au concentration products in the present invention Fig. 12Te3Thermoelectric material ESEM shape appearance figure.
Sb synthesized when being 0.5%Au concentration products in the present invention Fig. 22Te3Thermoelectric material ESEM shape appearance figure.
Sb synthesized when being 2%Au concentration products in the present invention Fig. 32Te3Thermoelectric material ESEM shape appearance figure.
Sb synthesized when being 4%Au concentration products in the present invention Fig. 42Te3Thermoelectric material ESEM shape appearance figure.
Fig. 5 is the Sb synthesized by the present invention2Te3Thermoelectric material thermoelectric material XRD facies analysis figures.
Fig. 6 is the Sb synthesized by the present invention2Te3The ZT value measurement result figures of thermoelectric material thermoelectric material.
Embodiment
Below in conjunction with brief description of the drawings, the present invention is described in further detail with embodiment.
A kind of gold nano grain cladding nanometer chip architecture Sb2Te3The preparation method of thermoelectric material, it is reduced by citric acid HAuCl4Method Au nano particles are reverted into Sb2Te3Surface on, some Au nano particles are in Sb2Te3The surface of nanometer sheet Coat very thin one layer, it is other some be embedded in the corner of hexagonal piece, lead to so as to build the conduction between different nanoscale twins Road and bridge, metal-semiconductor hetero-junctions is formed, so as to improve the pure phase hexagonal nanometer obtained by conventional solvent thermal synthesis method Chip architecture Sb2Te3ZT values.In hexagonal nanometer chip architecture Sb2Te3On the premise of the synthesis condition of thermoelectric material, ZT values are fixed, Pure phase hexagonal nanometer chip architecture Sb can be effectively lifted using this method2Te3ZT values：When gold content is controlled 1% (1% Au@Sb2Te3, i.e. Au and binary pure phase Sb2Te3Mass ratio is 1%) best results, ZT values and hexagonal nanometer chip architecture Sb2Te3 Thermoelectric material, which is compared, can lift 1.3 times.Specifically include following step：
Step 1, binary pure phase Sb is made using solvent-thermal method2Te3Powder, it is then centrifuged for washing and drying, and ESEM Its pattern is observed, confirms as a nanometer chip architecture.
Step 2, configure 0.01mol/L HAuCl4(gold chloride) aqueous solution.
Step 3, configure 0.1%wt AgNO3(silver nitrate) aqueous solution.
Step 4, configure 0.1%wt Na3C6H5O7(sodium citrate) aqueous solution.
Step 5, in the aqueous solution of 100ml boilings, sequentially add 1ml HAuCl4, 20~40 μ lAgNO3With 1~6ml Na3C6H5O7Mixed liquor, and 0.197 gram of Sb2Te3Powder, and stir.
Step 6, the mixed liquor in step 5 reacts under fluidized state to be stopped heating after 15min and carries out natural cooling；For Ensure the gold nano grain in Sb2Te3Uniformly coated in nanometer sheet, in cooling procedure keep reaction solution is persistently stirred it is 2 small When, last centrifuge washing drying, so as to obtain powdered product 1%Au@Sb2Te3。
Referring to Fig. 1 to Fig. 6, SEM morphology characterizations, it was found from Fig. 1 to Fig. 4, Au particles and Sb are carried out to product2Te3Nanometer sheet Between heterogeneous distribution knot it is high-visible.XRD phase composition signs, as can be seen from Figure 5, Sb are carried out to product2Te3Thermoelectric material phase group As simple substance Au+ binary pure phases Sb2Te3Composite.Product powder sintering is surveyed into progress thermoelectricity capability ZT values after block Amount, as can be seen from Figure 6, in 500K, 1%Au@Sb2Te3ZT values reach 0.8, compared to binary pure phase Sb2Te3ZT values 0.35 carry 1.3 times are risen.
Embodiment one：
Step 1, binary pure phase Sb is made using solvent-thermal method2Te3Powder, centrifuge washing drying, and scanning electron microscopic observation Its pattern, confirm as a nanometer chip architecture.
Step 2, configure 0.01mol/L HAuCl4(gold chloride) aqueous solution.
Step 3, configure 0.1%wt AgNO3(silver nitrate) aqueous solution.
Step 4, configure 0.1%wt Na3C6H5O7(sodium citrate) aqueous solution.
Step 5, in the aqueous solution of 100ml boilings, sequentially add 1ml HAuCl4、20μlAgNO3And 1ml Na3C6H5O7Mixed liquor, and 0.197 gram of Sb2Te3Powder, and stir.
Step 6, the mixed liquor in step 5 reacts under fluidized state to be stopped heating after 15min and carries out natural cooling, is Ensure the gold nano grain in Sb2Te3Uniformly coated in nanometer sheet, in cooling procedure keep reaction solution is persistently stirred it is 2 small When, last centrifuge washing drying, so as to obtain powdered product 1%Au@Sb2Te3。
Embodiment two：
Step 1, binary pure phase Sb is made using solvent-thermal method2Te3Powder, centrifuge washing drying, and scanning electron microscopic observation Its pattern, confirm as a nanometer chip architecture.
Step 2, configure 0.01mol/L HAuCl4(gold chloride) aqueous solution.
Step 3, configure 0.1%wt AgNO3(silver nitrate) aqueous solution.
Step 4, configure 0.1%wt Na3C6H5O7(sodium citrate) aqueous solution.
Step 5, in the aqueous solution of 100ml boilings, sequentially add 1ml HAuCl4、30μlAgNO3And 3ml Na3C6H5O7Mixed liquor, and 0.197 gram of Sb2Te3Powder, and stir.
Step 6, the mixed liquor in step 5 reacts under fluidized state to be stopped heating after 15min and carries out natural cooling, is Ensure the gold nano grain in Sb2Te3Uniformly coated in nanometer sheet, in cooling procedure keep reaction solution is persistently stirred it is 2 small When, last centrifuge washing drying, so as to obtain powdered product 1%Au@Sb2Te3。
Embodiment three：
Step 1, binary pure phase Sb is made using solvent-thermal method2Te3Powder, centrifuge washing drying, and scanning electron microscopic observation Its pattern, confirm as a nanometer chip architecture.
Step 2, configure 0.01mol/L HAuCl4(gold chloride) aqueous solution.
Step 3, configure 0.1%wt AgNO3(silver nitrate) aqueous solution.
Step 4, configure 0.1%wt Na3C6H5O7(sodium citrate) aqueous solution.
Step 5, in the aqueous solution of 100ml boilings, sequentially add 1ml HAuCl4、40μlAgNO3And 6ml Na3C6H5O7Mixed liquor, and 0.197 gram of Sb2Te3Powder, and stir.
Step 6, the mixed liquor in step 5 reacts under fluidized state to be stopped heating after 15min and carries out natural cooling, is Ensure the gold nano grain in Sb2Te3Uniformly coated in nanometer sheet, in cooling procedure keep reaction solution is persistently stirred it is 2 small When, last centrifuge washing drying, so as to obtain powdered product 1%Au@Sb2Te3。
The nanometer chip architecture Sb that the present invention obtains solvent structure2Te3Powder is dispersed in specific solvent, by molten Chemical reaction between agent generates gold nano grain, and then gold grain is attached to scattered nanometer sheet surface in a solvent immediately, from And form nano particle cladding nanometer chip architecture；So as to effectively lift pure phase nanometer chip architecture Sb2Te3Thermoelectric figure of merit, using gold The compound Sb obtained after nano particle cladding nanometer sheet2Te3Thermoelectric material ZT values compared with original structure can lift more than 1 times.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention, On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, said structure should be all considered as belonging to Protection scope of the present invention.

Claims (1)

  1. A kind of 1. gold nano grain cladding nanometer chip architecture Sb2Te3The preparation method of thermoelectric material, it is characterised in that including following The step of：
    Step 1, binary pure phase Sb is made using solvent-thermal method2Te3Powder, it is then centrifuged for washing and drying, and scanning electron microscopic observation Its pattern, confirm as a nanometer chip architecture；
    Step 2, configure 0.01mol/L HAuCl4The aqueous solution；
    Step 3, configure 0.1%wt AgNO3The aqueous solution；
    Step 4, configure 0.1%wt Na3C6H5O7The aqueous solution；
    Step 5, in the aqueous solution of 100ml boilings, sequentially add 1ml HAuCl4、20~40μl AgNO3With 1 ~ 6ml Na3C6H5O7Mixed liquor, and 0.197 gram of Sb2Te3Powder, and stir；
    Step 6, the mixed liquor in step 5 reacts under fluidized state to be stopped heating after 15min and carries out natural cooling, is being cooled down During keep persistently stirring reaction solution 2 hours, last centrifuge washing drying, so as to obtain powdered product 1%Au@ Sb2Te3。
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CN109659427A (en) * 2018-12-14 2019-04-19 昆明理工大学 A kind of transition metal cladding In2O3(ZnO)5The preparation method of nucleocapsid structure thermoelectric material
US20200013939A1 (en) * 2017-02-16 2020-01-09 Wake Forest University Composite nanoparticle compositions and assemblies
CN112670502A (en) * 2021-01-28 2021-04-16 河南工业大学 Antimony telluride nanosheet and application thereof in water-based zinc ion battery

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20200013939A1 (en) * 2017-02-16 2020-01-09 Wake Forest University Composite nanoparticle compositions and assemblies
US11631795B2 (en) * 2017-02-16 2023-04-18 Wake Forest University Nanocomposite comprising semiconductor and metal nanoparticles, and assemblies
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CN112670502A (en) * 2021-01-28 2021-04-16 河南工业大学 Antimony telluride nanosheet and application thereof in water-based zinc ion battery
CN112670502B (en) * 2021-01-28 2022-11-18 河南工业大学 Antimony telluride nanosheet and application thereof in water-based zinc ion battery

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