CN108275674B - Super-elastic graphene aerogel with thermoelectric effect and preparation method thereof - Google Patents
Super-elastic graphene aerogel with thermoelectric effect and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a thermoelectric effectThe super-elastic graphene aerogel and the preparation method thereof have a two-stage framework structure, wherein the first-stage framework is a polyurethane fiber network, and the second-stage framework is a three-dimensional network formed by active thermoelectric materials. The preparation method comprises the following steps: sb2Te3Dispersing the two-dimensional nanosheets in deionized water, stirring and ultrasonically treating to obtain Sb2Te3A two-dimensional nanosheet dispersion; dispersing graphite oxide in the dispersion liquid, stirring and carrying out ultrasonic treatment to obtain graphene oxide/Sb2Te3A two-dimensional nanosheet composite dispersion; immersing the pretreated polyurethane foam into the composite dispersion liquid, performing ultrasonic immersion adsorption, and freeze-drying to obtain graphene oxide aerogel; reducing, washing, and freeze-drying. The graphene aerogel disclosed by the invention can convert heat energy in the environment into electric energy, provides energy for microelectronic devices, and has an important application prospect in wearable fields such as medical monitoring and intelligent clothing.
Description
Technical Field
The invention belongs to the technical field of thermoelectric materials, and particularly relates to a super-elastic graphene aerogel with a thermoelectric effect and a preparation method thereof.
Background
The thermoelectric material refers to a functional material capable of converting thermal energy and electric energy into each other. Thermoelectric material thermoelectric power generation and power-on refrigeration methodThe method has very wide research and application prospects, and is mainly applied to automobile exhaust waste heat power generation, industrial waste heat recycling, deep-sea detectors in deep space and solar efficient photo-thermal-electric integrated systems at present. Thermoelectric materials have the property of converting waste heat into electric energy, and are drawing increasing attention. So far, Bi of high conversion efficiency2Te3Ceramics, flexible conductive polymer thermoelectric devices and a series of highly conductive carbon nanomaterial thermoelectric devices are developed successively.
With the development of intelligent wearable equipment, the energy supply problem becomes a problem to be solved urgently. Compared with a flexible solar cell, the thermoelectric material has the advantage of being not limited by the external environment, so the research and development of the thermoelectric material, particularly the elastic thermoelectric material, are greatly concerned. The elastic thermoelectric material can directly convert heat energy into electric energy while conducting human body heat so as to supply energy to the wearable device. However, the problems of low conversion efficiency and poor elasticity of the conventional flexible thermoelectric material generally exist, so that the improvement of the conversion efficiency and the elasticity of the thermoelectric material is urgent.
Disclosure of Invention
The technical problem to be solved by the invention is to provide the super-elastic graphene aerogel with the thermoelectric effect and the preparation method thereof, and the prepared super-elastic graphene aerogel can convert heat energy into electric energy and has high-efficiency and stable thermoelectric conversion efficiency.
The super-elastic graphene aerogel with the thermoelectric effect has a two-stage framework structure, wherein a first-stage framework is a polyurethane fiber network, and a second-stage framework is a three-dimensional network formed by active thermoelectric materials.
The invention discloses a preparation method of a super-elastic graphene aerogel with a thermoelectric effect, which comprises the following steps:
(1) sb2Te3Dispersing the two-dimensional nanosheets in deionized water, stirring and ultrasonically treating to obtain Sb with the concentration of 1.00-2.50 mg/ml2Te3A two-dimensional nanosheet dispersion;
(2) dispersing graphite oxide in the dispersion liquid obtained in the step (1), stirring and performing ultrasonic treatment to obtain oxygen with the concentration of 10-25 mg/mlgraphene/Sb alloy2Te3A two-dimensional nanosheet composite dispersion;
(3) immersing the pretreated polyurethane foam into the composite dispersion liquid obtained in the step (2), performing ultrasonic immersion adsorption, and freeze-drying to obtain graphene oxide aerogel;
(4) and (4) reducing the graphene oxide aerogel obtained in the step (3), washing, freezing and drying to obtain the super-elastic graphene aerogel with the thermoelectric effect.
The stirring in the step (1) is magnetic stirring, and the magnetic stirring time is 20-50 min; the ultrasound is water bath ultrasound, and the water bath ultrasound time is 30-60 min.
The stirring in the step (2) is magnetic stirring, and the magnetic stirring time is 20-50 min; the ultrasound is water bath ultrasound, and the water bath ultrasound time is 72-90 h.
The process conditions for pretreating the polyurethane foam in the step (3) are as follows: and respectively and alternately washing the mixture for 2 to 5 times by using deionized water and ethanol and drying the mixture.
The technological parameters of ultrasonic dipping adsorption in the step (3) are as follows: the dipping time is 10-25 min, and the ultrasonic intensity is 20-50W.
The freeze drying process parameters in the step (3) are as follows: the freezing temperature is-5 to-196 ℃, the freezing time is 0.1 to 24 hours, the vacuum degree of freeze drying is 5 to 20Pa, and the freeze drying time is 48 to 84 hours.
The reduction process conditions in the step (4) are as follows: and (3) heating an ascorbic acid solution with the concentration of 30-75 mg/ml to 75-90 ℃, preserving heat for 10-25 min, and then reducing the graphene oxide aerogel for 1-4 h.
The washing process conditions in the step (4) are as follows: soaking in absolute ethyl alcohol for 2-5 h, and repeatedly washing for 2-5 times.
The freeze drying process parameters in the step (4) are as follows: the vacuum degree of freeze drying is 5-20 Pa, and the freeze drying time is 48-84 h.
The invention is realized by changing Sb2Te3The concentrations of the two-dimensional nanosheets and the graphite oxide dispersion liquid and the water bath ultrasonic and freeze drying time can be used for realizing the internal treatment of the hyperelastic graphene aerogelAnd (3) regulation and control of an active thermoelectric three-dimensional network structure. The obtained graphene aerogel with the double-support framework structure has the high conductivity of graphene, has a macroporous structure of polyurethane foam, and has a great application prospect in flexible wearable self-powered equipment.
The hyperelastic graphene aerogel prepared by the invention has higher thermoelectric conversion efficiency mainly because the graphene has excellent electrical conductivity, the multiphase interface formed by the porous structure of the foam reduces the thermal conductivity of the graphene aerogel, and Sb filled in the porous structure of the graphene aerogel2Te3The two-dimensional nanosheets enhance the thermoelectric conversion efficiency of the graphene aerogel.
Advantageous effects
(1) The invention realizes the elasticization of the traditional thermoelectric material and provides a solution for the heat energy capture of curved surface machinery and limited space.
(2) The super-elastic graphene aerogel prepared by the invention has a three-dimensional network porous structure, and compared with other three-dimensional thermoelectric materials, the thermoelectric conversion efficiency is remarkably improved.
(3) The preparation method is simple in preparation process, environment-friendly, pollution-free, suitable for industrial production and low in cost.
Drawings
Fig. 1 is a digital photograph of the superelastic graphene aerogel in example 1 rebounded under finger pressure; wherein be the graphite alkene aerogel before pressing from a left side to the right side in proper order, graphite alkene aerogel when pressing, the graphite alkene aerogel after kick-backing.
Fig. 2 is a scanning electron microscope image of the superelastic graphene aerogel in example 2; the left image is a scanning electron microscope image of the graphene aerogel with the porous structure, and the right image is a scanning electron microscope image of the graphene-coated polyurethane fiber.
FIG. 3 shows Sb in example 32Te3Scanning electron microscope images of the two-dimensional nanoplates.
Fig. 4 is a graph (top) of the open-circuit voltage generated by the superelastic graphene aerogel in example 4 when the temperature difference exists and a corresponding graph (bottom) of the temperature rise and fall.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) 100mg of Sb was weighed2Te3Dispersing the two-dimensional nano-sheets in 100ml of deionized water, magnetically stirring for 20min, and performing water bath ultrasound for 30min to obtain Sb with the concentration of 1.00mg/ml2Te3A two-dimensional nanoplate dispersion.
(2) Weighing 1.00g of graphite oxide dispersed in Sb obtained in the step (1)2Te3In the two-dimensional nano-sheet dispersion liquid, magnetically stirring for 20min, and performing water bath ultrasound for 72h to obtain uniform and stable graphene oxide/Sb with the concentration of 10mg/ml2Te3Two-dimensional nano-sheet composite dispersion.
(3) Pretreating polyurethane foam, sequentially and alternately washing with deionized water and ethanol for 2 times and drying, and then soaking pretreated polyurethane foam into the graphene oxide/Sb obtained in the step (2)2Te3Performing ultrasonic immersion adsorption in the two-dimensional nanosheet composite dispersion liquid, wherein the immersion time is 10min, the ultrasonic intensity is 20W, taking out, and adsorbing the graphene oxide/Sb2Te3And (2) freezing the polyurethane foam of the two-dimensional nanosheet composite dispersion liquid in an environment at-5 ℃ for 24h, then quickly taking the frozen polyurethane foam out of liquid nitrogen, putting the polyurethane foam into a vacuum freeze dryer, and carrying out vacuum freeze drying for 48h under the condition that the vacuum degree is 5Pa to obtain the graphene oxide aerogel.
(4) Preparing an ascorbic acid solution with the concentration of 30mg/ml, heating to 75 ℃, preserving heat for 10min, placing the graphene oxide aerogel obtained in the step (3) in the ascorbic acid solution with the temperature of 75 ℃ for reduction for 1h, then soaking in absolute ethyl alcohol for 2h, repeatedly washing for 2 times, and then placing in a freeze dryer for drying, wherein the vacuum degree is 5Pa, and the freeze drying time is 48h, so as to obtain the super-elastic graphene aerogel with the thermoelectric effect.
The graphene aerogel prepared by the embodiment has a two-stage framework structure, wherein the first-stage framework is a polyurethane fiber network, and the second-stage framework is a three-dimensional network formed by active thermoelectric materials.
Fig. 1 is a digital photograph of the superelastic graphene aerogel under finger pressure, and it can be seen that: the super-elastic graphene aerogel can be compressed to the height of 20% under the large-force pressing force of fingers; when the fingers are released, the super-elastic graphene aerogel can recover to the height of more than 98% of the super-elastic graphene aerogel within 5 seconds. The super-elastic graphene aerogel prepared by the method has very excellent compression performance and rebound resilience, and the conductivity is unchanged after rebound.
The thermoelectric effect performance test of the graphene aerogel prepared in this embodiment is performed, and it can be known through the test and calculation that the Seebeck value S of the graphene aerogel in this embodiment is 22 μ V/K.
Example 2
(1) 150mg of Sb was weighed2Te3Dispersing the two-dimensional nano-sheets in 100ml of deionized water, magnetically stirring for 30min, and performing water bath ultrasound for 40min to obtain Sb with the concentration of 1.50mg/ml2Te3A two-dimensional nanoplate dispersion.
(2) 1.50g of graphite oxide is weighed and dispersed in the Sb obtained in the step (1)2Te3Magnetically stirring the two-dimensional nanosheet dispersion liquid for 30min, and performing water bath ultrasound for 78h to obtain uniform and stable graphene oxide/Sb with the concentration of 15mg/ml2Te3Two-dimensional nano-sheet composite dispersion.
(3) Pretreating polyurethane foam, sequentially and alternately washing with deionized water and ethanol for 3 times and drying, and then soaking pretreated polyurethane foam into the graphene oxide/Sb obtained in the step (2)2Te3Performing ultrasonic immersion adsorption in the two-dimensional nanosheet composite dispersion liquid, wherein the immersion time is 15min, the ultrasonic intensity is 30W, taking out, and adsorbing the graphene oxide/Sb2Te3The polyurethane foam of the two-dimensional nano-sheet composite dispersion liquid is placed in an environment with the temperature of-60 ℃ for freezing for 16h, and then the frozen polyurethane foam is rapidly frozenThe polyurethane foam is taken out from the liquid nitrogen and then placed in a vacuum freeze dryer, and the vacuum freeze drying is carried out for 60 hours under the condition that the vacuum degree is 10Pa, so as to obtain the graphene oxide aerogel.
(4) Preparing an ascorbic acid solution with the concentration of 45mg/ml, heating to 80 ℃, preserving heat for 15min, placing the graphene oxide aerogel obtained in the step (3) in the ascorbic acid solution with the temperature of 80 ℃ for reduction for 2h, then soaking in absolute ethyl alcohol for 3h, repeatedly washing for 3 times, and then placing in a freeze dryer for drying, wherein the vacuum degree is 10Pa, and the freeze drying time is 60h, so as to obtain the super-elastic graphene aerogel with the thermoelectric effect.
The graphene aerogel prepared by the embodiment has a two-stage framework structure, wherein the first-stage framework is a polyurethane fiber network, and the second-stage framework is a three-dimensional network formed by active thermoelectric materials.
Fig. 2 is a Scanning Electron Microscope (SEM) image of the superelastic graphene aerogel prepared in this example, and it can be seen that: in the left picture, the graphene sheets are embedded in holes among polyurethane fibers, Sb2Te3The two-dimensional nanosheets are used as fillers and inserted between the graphene lamella layers and embedded on the surface of the graphene lamella layers; in the right picture, the graphene sheet layer is tightly coated on the surface of the polyurethane fiber, wherein Sb2Te3The two-dimensional nano-sheets are filled between the graphene sheet layers and the polyurethane fibers.
The thermoelectric effect and the elastic property of the graphene aerogel prepared in the embodiment are tested, and the test and calculation show that the graphene aerogel in the embodiment can be compressed to 22% of the height of the graphene aerogel, and can instantly recover 97.6% of the height of the graphene aerogel within 6 s; the Seebeck value S of the graphene aerogel is 24 mu V/K.
Example 3
(1) Weighing 200mg of Sb2Te3Dispersing the two-dimensional nano-sheets in 100ml of deionized water, magnetically stirring for 40min, and performing water bath ultrasound for 50min to obtain Sb with the concentration of 2.00mg/ml2Te3A two-dimensional nanoplate dispersion.
(2) Weighing 2.00g of graphite oxide dispersed in Sb obtained in the step (1)2Te3Magnetic stirring in two-dimensional nanosheet dispersionStirring for 40min, and performing water bath ultrasound for 84h to obtain uniform and stable graphene oxide/Sb with the concentration of 20mg/ml2Te3Two-dimensional nano-sheet composite dispersion.
(3) Pretreating polyurethane foam, sequentially and alternately washing with deionized water and ethanol for 4 times and drying, and then soaking pretreated polyurethane foam into the graphene oxide/Sb obtained in the step (2)2Te3Performing ultrasonic immersion adsorption in the two-dimensional nanosheet composite dispersion liquid, wherein the immersion time is 20min, the ultrasonic intensity is 40W, taking out, and adsorbing the graphene oxide/Sb2Te3And (2) freezing the polyurethane foam of the two-dimensional nanosheet composite dispersion liquid for 8h in an environment at-120 ℃, then quickly taking the frozen polyurethane foam out of liquid nitrogen, putting the polyurethane foam into a vacuum freeze dryer, and carrying out vacuum freeze drying for 72h under the condition that the vacuum degree is 15Pa to obtain the graphene oxide aerogel.
(4) Preparing an ascorbic acid solution with the concentration of 60mg/ml, heating to 85 ℃, preserving heat for 20min, placing the graphene oxide aerogel obtained in the step (3) in the ascorbic acid solution with the temperature of 85 ℃ for reduction for 3h, then soaking in absolute ethyl alcohol for 4h, repeatedly washing for 4 times, and then placing in a freeze dryer for drying, wherein the vacuum degree is 15Pa, and the freeze drying time is 72h, so as to obtain the super-elastic graphene aerogel with the thermoelectric effect.
The graphene aerogel prepared by the embodiment has a two-stage framework structure, wherein the first-stage framework is a polyurethane fiber network, and the second-stage framework is a three-dimensional network formed by active thermoelectric materials.
FIG. 3 shows Sb in this example2Te3Electron Microscopy (SEM) of the two-dimensional nanoplatelets, it can be seen that: sb2Te3The two-dimensional nano-sheet is of a quasi-regular hexagon structure.
The thermoelectric effect and the elasticity performance of the graphene aerogel prepared by the embodiment are tested, and the test and calculation show that the graphene aerogel can be compressed to 24% of the height of the graphene aerogel and can instantly recover to 97.2% of the height of the graphene aerogel within 7 s; the Seebeck value S of the graphene aerogel is 26 mu V/K.
Example 4
(1) Weighing 250mg of Sb2Te3Dispersing the two-dimensional nano-sheets in 100ml of deionized water, magnetically stirring for 50min, and ultrasonically treating in water bath for 60min to obtain Sb with the concentration of 2.50mg/ml2Te3A two-dimensional nanoplate dispersion.
(2) 2.50g of graphite oxide is weighed and dispersed in the Sb obtained in the step (1)2Te3Magnetically stirring the two-dimensional nanosheet dispersion liquid for 50min, and performing water bath ultrasound for 90h to obtain uniform and stable graphene oxide/Sb with the concentration of 25mg/ml2Te3Two-dimensional nano-sheet composite dispersion.
(3) Pretreating polyurethane foam, sequentially and alternately washing with deionized water and ethanol for 5 times and drying, and then soaking pretreated polyurethane foam into the graphene oxide/Sb obtained in the step (2)2Te3Performing ultrasonic impregnation and adsorption in the two-dimensional nanosheet composite dispersion liquid, wherein the impregnation time is 25min, the ultrasonic intensity is 50W, taking out, and adsorbing the graphene oxide/Sb2Te3And (2) freezing the polyurethane foam of the two-dimensional nanosheet composite dispersion liquid for 0.1h in an environment at the temperature of-196 ℃, then quickly taking the frozen polyurethane foam out of liquid nitrogen, putting the polyurethane foam into a vacuum freeze dryer, and carrying out vacuum freeze drying for 84h under the condition that the vacuum degree is 20Pa to obtain the graphene oxide aerogel.
(4) Preparing an ascorbic acid solution with the concentration of 75mg/ml, heating to 90 ℃, preserving heat for 25min, placing the graphene oxide aerogel obtained in the step (3) in the ascorbic acid solution with the temperature of 90 ℃ for reduction for 3h, then soaking in absolute ethyl alcohol for 5h, repeatedly washing for 5 times, and then placing in a freeze dryer for drying, wherein the vacuum degree is 20Pa, and the freeze drying time is 84h, so as to obtain the super-elastic graphene aerogel with the thermoelectric effect.
The graphene aerogel prepared by the embodiment has a two-stage framework structure, wherein the first-stage framework is a polyurethane fiber network, and the second-stage framework is a three-dimensional network formed by active thermoelectric materials.
Fig. 4 is a graph (top) of open-circuit voltage generated by the superelastic graphene aerogel prepared in this example when the temperature difference is present and a corresponding temperature increase and decrease curve (bottom), and it can be seen that: when the temperature correspondingly rises and falls, the open-circuit voltage generated by the superelastic graphene aerogel rises along with the increase of the temperature difference, and the SeeBeck value is calculated to be 28 muV/K.
Elasticity performance test is carried out to the graphite alkene aerogel that this embodiment made, and through test and calculation can know, graphite alkene aerogel can compress to 26% of its height in this embodiment to can resume 97.0% of its height in the 8s in the twinkling of an eye.
Claims (10)
1. A preparation method of super-elastic graphene aerogel with thermoelectric effect comprises the following steps:
(1) sb2Te3Dispersing the two-dimensional nanosheets in deionized water, stirring and ultrasonically treating to obtain Sb with the concentration of 1.00-2.50 mg/ml2Te3A two-dimensional nanosheet dispersion;
(2) dispersing graphite oxide in the dispersion liquid obtained in the step (1), stirring, and performing ultrasonic treatment to obtain graphene oxide/Sb with the concentration of 10-25 mg/ml2Te3A two-dimensional nanosheet composite dispersion;
(3) immersing the pretreated polyurethane foam into the composite dispersion liquid obtained in the step (2), performing ultrasonic immersion adsorption, and freeze-drying to obtain graphene oxide aerogel;
(4) and (4) reducing the graphene oxide aerogel obtained in the step (3), washing, freezing and drying to obtain the super-elastic graphene aerogel with the thermoelectric effect.
2. The method for preparing the superelastic graphene aerogel with thermoelectric effect according to claim 1, wherein the method comprises the following steps: the stirring in the step (1) is magnetic stirring, and the magnetic stirring time is 20-50 min; the ultrasound is water bath ultrasound, and the water bath ultrasound time is 30-60 min.
3. The method for preparing the superelastic graphene aerogel with thermoelectric effect according to claim 1, wherein the method comprises the following steps: the stirring in the step (2) is magnetic stirring, and the magnetic stirring time is 20-50 min; the ultrasound is water bath ultrasound, and the water bath ultrasound time is 72-90 h.
4. The method for preparing the superelastic graphene aerogel with thermoelectric effect according to claim 1, wherein the method comprises the following steps: the process conditions for pretreating the polyurethane foam in the step (3) are as follows: and respectively and alternately washing the mixture for 2 to 5 times by using deionized water and ethanol and drying the mixture.
5. The method for preparing the superelastic graphene aerogel with thermoelectric effect according to claim 1, wherein the method comprises the following steps: the technological parameters of ultrasonic dipping adsorption in the step (3) are as follows: the dipping time is 10-25 min, and the ultrasonic intensity is 20-50W.
6. The method for preparing the superelastic graphene aerogel with thermoelectric effect according to claim 1, wherein the method comprises the following steps: the freeze drying process parameters in the step (3) are as follows: the freezing temperature is-5 to-196 ℃, the freezing time is 0.1 to 24 hours, the vacuum degree of freeze drying is 5 to 20Pa, and the freeze drying time is 48 to 84 hours.
7. The method for preparing the superelastic graphene aerogel with thermoelectric effect according to claim 1, wherein the method comprises the following steps: the reduction process conditions in the step (4) are as follows: and (3) heating an ascorbic acid solution with the concentration of 30-75 mg/ml to 75-90 ℃, preserving heat for 10-25 min, and then reducing the graphene oxide aerogel for 1-4 h.
8. The method for preparing the superelastic graphene aerogel with thermoelectric effect according to claim 1, wherein the method comprises the following steps: the washing process conditions in the step (4) are as follows: soaking in absolute ethyl alcohol for 2-5 h, and repeatedly washing for 2-5 times.
9. The method for preparing the superelastic graphene aerogel with thermoelectric effect according to claim 1, wherein the method comprises the following steps: the freeze drying process parameters in the step (4) are as follows: the vacuum degree of freeze drying is 5-20 Pa, and the freeze drying time is 48-84 h.
10. The super-elastic graphene aerogel with thermoelectric effect, prepared by the method according to any one of claims 1 to 9, is characterized in that: the composite material has a two-stage framework structure, wherein the first-stage framework is a polyurethane fiber network, and the second-stage framework is a three-dimensional network formed by active thermoelectric materials.
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| CN102760827A (en) * | 2012-07-23 | 2012-10-31 | 浙江大学 | Bi2Te3 thin-piece/graphene composite material, preparation method and applications thereof |
| US8852444B2 (en) * | 2009-08-14 | 2014-10-07 | Northwestern University | Sorting two-dimensional nanomaterials by thickness |
| WO2017060719A1 (en) * | 2015-10-08 | 2017-04-13 | The University Of Manchester | Aerogels |
| CN106809822A (en) * | 2017-01-22 | 2017-06-09 | 戴天元 | A kind of preparation method of super-elasticity graphene aerogel |
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| US8852444B2 (en) * | 2009-08-14 | 2014-10-07 | Northwestern University | Sorting two-dimensional nanomaterials by thickness |
| CN102760827A (en) * | 2012-07-23 | 2012-10-31 | 浙江大学 | Bi2Te3 thin-piece/graphene composite material, preparation method and applications thereof |
| WO2017060719A1 (en) * | 2015-10-08 | 2017-04-13 | The University Of Manchester | Aerogels |
| CN106809822A (en) * | 2017-01-22 | 2017-06-09 | 戴天元 | A kind of preparation method of super-elasticity graphene aerogel |
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