CN106505142A - A kind of preparation method of flexible N-type telluride nano silver wire thermal electric film - Google Patents
A kind of preparation method of flexible N-type telluride nano silver wire thermal electric film Download PDFInfo
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- CN106505142A CN106505142A CN201610831800.7A CN201610831800A CN106505142A CN 106505142 A CN106505142 A CN 106505142A CN 201610831800 A CN201610831800 A CN 201610831800A CN 106505142 A CN106505142 A CN 106505142A
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- silver
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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
- H10N10/852—Thermoelectric active materials comprising inorganic compositions comprising tellurium, selenium or sulfur
Abstract
The invention discloses a kind of preparation method of flexible N-type telluride nano silver wire thermal electric film, the method is comprised the following steps：Telluride nano silver wire is mixed with polyvinylpyrrolidone, ultrasonic disperse obtains silver telluride nanowire dispersion in a solvent；Under conditions of vacuum filtration, by uniform for silver telluride nanowire dispersion drop coating on glass fiber filter, obtain sticking to the silver telluride nano wire film on glass fiber filter in 75 DEG C of vacuum dryings；It is sandwiched between two copy papers, is positioned over extrusion molding in tablet machine, then remove the glass fiber filter fragment at the silver telluride nano wire film back side with brush, is placed in annealing in vacuum drying oven and obtains target product.Of the invention simply controllable, short preparation period, safety non-pollution, energy consumption is low, the thin film thermoelectric excellent performance that obtains, flexible good, the flexible thermal electric film of different size and shape neatly can be prepared according to the size and shape of glass fibre membrane, had broad application prospects.
Description
Technical field：
The present invention relates to novel energy resource material technology field, and in particular to a kind of flexible N-type telluride nano silver wire thermal electric film
Preparation method.
Background technology：
Electric energy directly mutually can be changed by thermoelectric material with heat energy, using thermoelectric material manufacture thermoelectric power generation device and
The features such as refrigeration device, energy discarded with noiselessness, pollution-free, recoverable when compact equipment, operation, in army
The fields such as thing, medical science, space flight, microelectronics or even household electrical appliance suffer from wide application prospect.Business compared by flexible thermoelectric material
The block thermoelectric material of industry, process is simple, the unique advantage such as applied widely little with flexible, weight, attracts in recent years
Scientific research circle and business circles are more and more paid close attention to.
Silver telluride synthesis is simple, with higher electrical conductivity and Seebeck coefficient, dispersibles after surfactant process
In water, it is suitable for preparing flexible thermoelectric material.But it is so far, by containing tellurium based on the flexible thermoelectric material of silver telluride
Prepared by the composite for changing silver nano-grain, preparation process is complicated, relatively costly, flexible poor.
Content of the invention：
It is an object of the invention to provide a kind of preparation method of flexible N-type telluride nano silver wire thermal electric film, the method work
Skill is simple, and short preparation period, safety non-pollution, energy consumption are low, the thin film thermoelectric excellent performance for obtaining, flexible good.
The present invention is achieved by the following technical programs：
A kind of preparation method of flexible N-type telluride nano silver wire thermal electric film, the method are comprised the following steps：
(1) telluride nano silver wire is mixed with polyvinylpyrrolidone, ultrasonic disperse obtains telluride in ethylene glycol solvent
Nano silver wire dispersion liquid；The concentration of telluride nano silver wire is 4-8mg/mL, and polyvinylpyrrolidoneconcentration concentration is 0.3-1mg/mL；
(2) under conditions of vacuum filtration, the uniform drop coating of silver telluride nanowire dispersion that step (1) is obtained is in glass
On fibrous filter membrane, the drop coating amount of silver telluride dispersion liquid is 0.4-1.6mL/cm2, after liquid is drained, obtain in 75 DEG C of vacuum dryings
To the silver telluride nano wire film sticked on glass fiber filter；
(3) the silver telluride nano wire film sticked on glass fiber filter that step (2) is obtained is clipped in two duplicating
Between paper, extrusion molding under 5-30Mpa is positioned in tablet machine, then removes the glass at the silver telluride nano wire film back side with brush
Glass fibrous filter membrane fragment, obtains the paper with silver telluride nano wire film；
(4) paper with silver telluride nano wire film that step (3) is obtained is placed in vacuum drying oven, 180-200 DEG C
Annealing 20-60 minutes obtain flexible N-type telluride nano silver wire thermal electric film.
Preferably, in step (1), the concentration of telluride nano silver wire is 4-6mg/mL, and polyvinylpyrrolidoneconcentration concentration is
0.3-0.5mg/mL.
Preferably, in step (2), the drop coating amount of silver telluride dispersion liquid is 0.6-1mL/cm2.
Preferably, in step (3), extrusion molding pressure is 10-30Mpa.
Preferably, in step (4), annealing temperature is 200 DEG C, and annealing time is 30-60 minutes.
Beneficial effects of the present invention are as follows：
1) present invention adds polyvinylpyrrolidone telluride nano silver wire to be dispersed in ethylene glycol and drop coating film forming, real
The flexibility of N-type telluride nano silver wire is showed while receiving to flexible N-type silver telluride by the concentration for controlling polyvinylpyrrolidone
The thermoelectricity capability of rice noodle thermal electric film is controlled.
2) present invention is by the extrusion molding to telluride Ag films and annealing so as to be transferred to from glass fiber filter
On common copy paper, the flexible and thermoelectricity capability of thin film is improve.
3) present invention process is simply controllable, short preparation period, safety non-pollution, energy consumption is low, the thin film thermoelectric performance that obtains
Excellent, flexible good.Required according to actual production, difference can be prepared according to the size and shape of glass fibre membrane neatly
Size and the flexible thermal electric film of shape, with wide prospects for commercial application.
Description of the drawings：
Fig. 1 is the silver telluride nano wire film sticked on glass fiber filter that 1 step 2 of the embodiment of the present invention is obtained
Electron scanning micrograph.
Fig. 2 is that the flexible N-type telluride nano silver wire thermoelectricity being attached on copy paper that 1 step 4 of the embodiment of the present invention is obtained is thin
The electron scanning micrograph of film.
Fig. 3 is the electricity for being attached to the flexible N-type telluride nano silver wire thermal electric film on copy paper that the embodiment of the present invention 1 is obtained
Conductance and power factor.
Fig. 4 is the electricity for being attached to the flexible N-type telluride nano silver wire thermal electric film on copy paper that the embodiment of the present invention 1 is obtained
Conductance and the relation for bending number of times.
Fig. 5 is the conductance of the silver telluride nano wire film sticked on glass fiber filter that comparative example of the present invention 1 is obtained
Rate and power factor.
Fig. 6 is the electricity for being attached to the flexible N-type telluride nano silver wire thermal electric film on copy paper that the embodiment of the present invention 2 is obtained
Conductance and power factor.
Fig. 7 is the electricity for being attached to the flexible N-type telluride nano silver wire thermal electric film on copy paper that the embodiment of the present invention 3 is obtained
Conductance and power factor.
Specific embodiment：
The following is and the present invention is further illustrated, rather than limitation of the present invention.
Embodiment 1：
(1) 30mg telluride nano silver wire and 1.5mg polyvinylpyrrolidones ultrasonic disperse are obtained in the ethylene glycol of 5mL
Arrive silver telluride nanowire dispersion；
(2) vacuum filtration auxiliary under, by uniform for the silver telluride nanowire dispersion of 0.75mL drop coating 2.5cm ×
On the glass fiber filter of 0.5cm, liquid is drained；The glass fiber filter that will be covered with telluride nano silver wire is true at 75 DEG C
Empty drying, obtains sticking to the silver telluride nano wire film on glass fiber filter, electron scanning micrograph such as Fig. 1 institutes
Show；
(3) the silver telluride nano wire film sticked on glass fiber filter that step (2) is obtained is clipped in two duplicating
Between paper, it is transferred in tablet machine, extrusion molding under 30MPa pressure, makes silver telluride nano wire film be transferred to a duplicating
The glass fiber filter fragment at the silver telluride nano wire film back side on paper, is then swept off with brush, is obtained with telluride silver nanoparticle
The paper of line thin film；
(4) finally the paper with silver telluride nano wire film that step (3) is obtained is placed in vacuum drying oven, in 200
At DEG C, annealing obtains the flexible N-type telluride nano silver wire thermal electric film being attached on copy paper, its scanning electron microscope for 30 minutes
Photo is as shown in Fig. 2 its electrical conductivity and power factor are as shown in figure 3, its electrical conductivity is as shown in Figure 4 with the relation of bending number of times.
By Fig. 1, Fig. 2 understands that, after 30MPa pressure extrusions, telluride nano silver wire is compressed together to form block accumulation, each other
Contact better, thin film more compacts, so as to there is higher electrical conductivity.As shown in Figure 4, the silver telluride being attached on copy paper is received
More preferably, 100 performances of bending are substantially unchanged for the flexibility of rice noodle thermal electric film, remain to keep more than 50% after bending 1000 times
Performance number.
Comparative example 1：
(1) 30mg telluride nano silver wire and 1.5mg polyvinylpyrrolidones ultrasonic disperse are obtained in the ethylene glycol of 5mL
Arrive silver telluride nanowire dispersion；
(2) vacuum filtration auxiliary under, by uniform for the silver telluride nanowire dispersion of 0.75mL drop coating 2.5cm ×
On the glass fiber filter of 0.5cm, liquid is drained；The glass fiber filter that will be covered with telluride nano silver wire is true at 75 DEG C
Empty drying, obtains sticking to the silver telluride nano wire film on glass fiber filter；
(3) the silver telluride nano wire film sticked on glass fiber filter that step (2) is obtained is placed in vacuum drying oven
In, annealing at 200 DEG C obtains flexible N-type telluride nano silver wire thermal electric film for 30 minutes, its electron scanning micrograph with
In embodiment 1, Fig. 1 is identical, and its electrical conductivity and power factor be shown in Fig. 5, due to glass fiber filter itself mechanical performance compared with
Difference, will fracture after bending fewer number (less than 10 times), therefore stick to the silver telluride nano wire film on glass fiber filter
Flexible poor.
The flexibility of the product obtained from embodiment 1 and comparative example 1, the present invention is more preferable, resistant to bending, electrical conductivity, power
The factor is higher, more has application prospect.
Embodiment 2：
(1) 35mg telluride nano silver wire and 3.5mg polyvinylpyrrolidones ultrasonic disperse are obtained in the ethylene glycol of 7mL
Arrive silver telluride nanowire dispersion；
(2) under vacuum filtration auxiliary, by uniform for the silver telluride nanowire dispersion of 1.0mL drop coating in 2.5cm × 0.5cm
Glass fiber filter on, liquid is drained；Will be covered with glass fiber filter vacuum baking at 75 DEG C of telluride nano silver wire
Dry, obtain sticking to the silver telluride nano wire film on glass fiber filter；
(3) the silver telluride nano wire film sticked on glass fiber filter that step (2) is obtained is clipped in two duplicating
Between paper, be transferred in tablet machine, extrusion molding under 10MPa pressure, then the silver telluride nano wire film back of the body is swept off with brush
The glass fiber filter fragment in face, obtains the paper with silver telluride nano wire film；
(4) finally the paper with silver telluride nano wire film that step (3) is obtained is placed in vacuum drying oven, in 200
At DEG C, annealing obtains the flexible N-type telluride nano silver wire thermal electric film being attached on copy paper for 20 minutes.Its electrical conductivity and power because
Sub as shown in Figure 6.
Embodiment 3：
(1) 40mg telluride nano silver wire and 10mg polyvinylpyrrolidones ultrasonic disperse are obtained in the ethylene glycol of 10mL
Arrive silver telluride nanowire dispersion；
(2) vacuum filtration auxiliary under, by uniform for the silver telluride nanowire dispersion of 0.90mL drop coating 2.5cm ×
On the glass fiber filter of 0.5cm, liquid is drained；The glass fiber filter that will be covered with telluride nano silver wire is true at 75 DEG C
Empty drying, obtains sticking to the silver telluride nano wire film on glass fiber filter；
(3) the silver telluride nano wire film sticked on glass fiber filter that step (2) is obtained is clipped in two duplicating
Between paper, be transferred in tablet machine, extrusion molding under 5MPa pressure, then the silver telluride nano wire film back side is swept off with brush
Glass fiber filter fragment, obtain the paper with silver telluride nano wire film；
(4) finally the paper with silver telluride nano wire film that step (3) is obtained is placed in vacuum drying oven, in 180
At DEG C, annealing obtains the flexible N-type telluride nano silver wire thermal electric film being attached on copy paper for 40 minutes.Its electrical conductivity and power because
Sub as shown in Figure 7.
Embodiment 4：
(1) 40mg telluride nano silver wire and 7.5mg polyvinylpyrrolidones ultrasonic disperse are obtained in the ethylene glycol of 10mL
Arrive silver telluride nanowire dispersion；
(2) under vacuum filtration auxiliary, by uniform for the silver telluride nanowire dispersion of 0.6mL drop coating in 2.5cm × 0.5cm
Glass fiber filter on, liquid is drained；Will be covered with glass fiber filter vacuum baking at 75 DEG C of telluride nano silver wire
Dry, obtain sticking to the silver telluride nano wire film on glass fiber filter；
(3) the silver telluride nano wire film sticked on glass fiber filter that step (2) is obtained is clipped in two duplicating
Between paper, be transferred in tablet machine, extrusion molding under 20MPa pressure, then the silver telluride nano wire film back of the body is swept off with brush
The glass fiber filter fragment in face, obtains the paper with silver telluride nano wire film；
(4) finally the paper with silver telluride nano wire film that step (3) is obtained is placed in vacuum drying oven, in 200
At DEG C, annealing obtains the flexible N-type telluride nano silver wire thermal electric film being attached on copy paper for 60 minutes.Work(at its 45 DEG C and 195 DEG C
The rate factor is respectively 76 μ W/ (mK2) and 143 μ W/ (mK2).
Embodiment 5：
(1) 20mg telluride nano silver wire and 3mg polyvinylpyrrolidones ultrasonic disperse are obtained in the ethylene glycol of 3mL
Silver telluride nanowire dispersion；
(2) under vacuum filtration auxiliary, by uniform for the silver telluride nanowire dispersion of 0.8mL drop coating in 2.5cm × 0.5cm
Glass fiber filter on, liquid is drained；Will be covered with glass fiber filter vacuum baking at 75 DEG C of telluride nano silver wire
Dry, obtain sticking to the silver telluride nano wire film on glass fiber filter；
(3) the silver telluride nano wire film sticked on glass fiber filter that step (2) is obtained is clipped in two duplicating
Between paper, be transferred in tablet machine, extrusion molding under 10MPa pressure, then the silver telluride nano wire film back of the body is swept off with brush
The glass fiber filter fragment in face, obtains the paper with silver telluride nano wire film；
(4) finally the paper with silver telluride nano wire film that step (3) is obtained is placed in vacuum drying oven, in 180
At DEG C, annealing obtains the flexible N-type telluride nano silver wire thermal electric film being attached on copy paper for 60 minutes.Work(at its 45 DEG C and 150 DEG C
The rate factor is respectively 65 μ W/ (mK2) and 115 μ W/ (mK2).
Claims (5)
1. a kind of preparation method of flexible N-type telluride nano silver wire thermal electric film, it is characterised in that the method includes following step
Suddenly：
(1) telluride nano silver wire is mixed with polyvinylpyrrolidone, ultrasonic disperse obtains silver telluride in ethylene glycol solvent and receives
Rice noodle dispersion liquid；The concentration of telluride nano silver wire is 4-8mg/mL, and polyvinylpyrrolidoneconcentration concentration is 0.3-1mg/mL；
(2) under conditions of vacuum filtration, the uniform drop coating of silver telluride nanowire dispersion that step (1) is obtained is in glass fibre
On filter membrane, the drop coating amount of silver telluride dispersion liquid is 0.4-1.6mL/cm2, after liquid is drained, glued in 75 DEG C of vacuum dryings
The silver telluride nano wire film being attached on glass fiber filter；
(3) by the silver telluride nano wire film sticked on glass fiber filter that step (2) is obtained be clipped in two copy papers it
Between, extrusion molding under 5-30Mpa is positioned in tablet machine, then removes the glass fibers at the silver telluride nano wire film back side with brush
Dimension filter membrane fragment, obtains the paper with silver telluride nano wire film；
(4) paper with silver telluride nano wire film that step (3) is obtained is placed in vacuum drying oven, 180-200 DEG C of annealing
20-60 minutes obtain flexible N-type telluride nano silver wire thermal electric film.
2. the preparation method of flexible N-type telluride nano silver wire thermal electric film according to claim 1, it is characterised in that step
Suddenly in (2), the drop coating amount of silver telluride dispersion liquid is 0.6-1mL/cm2.
3. the preparation method of flexible N-type telluride nano silver wire thermal electric film according to claim 1 and 2, it is characterised in that
In step (1), the concentration of telluride nano silver wire is 4-6mg/mL；Polyvinylpyrrolidoneconcentration concentration is 0.3-0.5mg/mL.
4. the preparation method of flexible N-type telluride nano silver wire thermal electric film according to claim 1 and 2, it is characterised in that
In step (3), extrusion molding pressure is 10-30Mpa.
5. the preparation method of flexible N-type telluride nano silver wire thermal electric film according to claim 1 and 2, it is characterised in that
In step (4), annealing temperature is 200 DEG C, and annealing time is 30-60 minutes.
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| CN110364616A (en) * | 2019-07-30 | 2019-10-22 | 中国科学院深圳先进技术研究院 | A kind of telluride silver nanowires flexible thermal conductive film and preparation method thereof welded at room temperature |
| CN111816753A (en) * | 2019-06-18 | 2020-10-23 | 桂林电子科技大学 | Preparation method of paper substrate bismuth telluride-based nanowire flexible thermocouple type temperature sensor |
| CN111864045A (en) * | 2020-06-30 | 2020-10-30 | 同济大学 | Method for preparing high-performance polyvinylpyrrolidone/silver selenide/nylon flexible composite thermoelectric film |
| CN112573558A (en) * | 2019-09-27 | 2021-03-30 | 上海大学 | Inorganic flexible thermoelectric material, method for producing same, and thermoelectric device provided with same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111816753B (en) * | 2019-06-18 | 2022-07-12 | 桂林电子科技大学 | Preparation method of paper substrate bismuth telluride-based nanowire flexible thermocouple type temperature sensor |
| CN110364616A (en) * | 2019-07-30 | 2019-10-22 | 中国科学院深圳先进技术研究院 | A kind of telluride silver nanowires flexible thermal conductive film and preparation method thereof welded at room temperature |
| CN112573558A (en) * | 2019-09-27 | 2021-03-30 | 上海大学 | Inorganic flexible thermoelectric material, method for producing same, and thermoelectric device provided with same |
| CN112573558B (en) * | 2019-09-27 | 2022-04-12 | 上海大学 | Inorganic flexible thermoelectric material, method for producing same, and thermoelectric device provided with same |
| CN111864045A (en) * | 2020-06-30 | 2020-10-30 | 同济大学 | Method for preparing high-performance polyvinylpyrrolidone/silver selenide/nylon flexible composite thermoelectric film |
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Application publication date: 20170315 Assignee: Guangxi Liaofan Instrument Equipment Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2022450000539 Denomination of invention: A Preparation Method of Flexible N-type Silver Telluride Nanowire Thermoelectric Thin Films Granted publication date: 20181123 License type: Common License Record date: 20221229 |
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