CN114574169A - Vanadium dioxide-boron nitride phase-change heat-conducting composite material and preparation method and application thereof - Google Patents
Vanadium dioxide-boron nitride phase-change heat-conducting composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a vanadium dioxide-boron nitride phase-change heat-conducting composite material and a preparation method and application thereof. The preparation method comprises the following steps: carrying out hydrothermal reaction on a vanadium salt, a reducing agent, boron nitride and a doping agent in a solvent; wherein the boron nitride is hexagonal boron nitride. According to the invention, a hydrothermal method is adopted to synthesize the vanadium dioxide-boron nitride phase-change heat-conducting composite material, and nano vanadium dioxide is adsorbed on the hexagonal boron nitride nanosheet. On one hand, vanadium dioxide endows the material with phase change heat storage capacity; on the other hand, through the electron-phonon coupling effect between the vanadium dioxide and the boron nitride, higher thermal conductivity is obtained under the condition of lower boron nitride loading capacity, the production cost is reduced, and meanwhile, the boron nitride has a protection effect on the vanadium dioxide, so that the thermal stability of the vanadium dioxide is improved. Compared with the prior art, the heat conduction oil has the advantages of no oil spilling phenomenon, good thermal stability and high heat conductivity coefficient.
Description
Technical Field
The invention relates to the technical field of chemical engineering, in particular to a vanadium dioxide-boron nitride phase-change heat-conducting composite material and a preparation method and application thereof.
Background
Phase Change Materials (PCM) are capable of changing the state of matter and providing latent heat at a constant temperature. The traditional organic phase-change material has the advantages of large phase-change enthalpy value, low cost, mild property, no problems of supercooling, corrosion and the like, low price and easiness in acquisition, and is a hotspot of research in the field of phase-change materials. However, the application of the organic phase-change material has two major difficulties, one is that the organic phase-change material mostly belongs to the category of solid-liquid phase-change materials, the material is in a liquid state after absorbing heat, the phase-change volume change is large, the phenomenon of oil spilling is easy to occur, and the thermal stability is poor; secondly, the thermal conductivity of the organic phase change material is generally small, generally 0.15-0.3W/(m.K), which affects the heat storage and release speed of the material and affects the use. Compared with organic phase change materials, the inorganic phase change materials have the characteristics of repeated use, no oil spill phenomenon, high reliability after long-term use and environmental protection, and have wide application prospects in the field of heat conduction materials. Wherein the vanadium dioxide is subjected to first-order reversible phase change at 68 ℃, has phase change heat storage capacity, has small volume change in the phase change process, and has intrinsic thermal conductivity of 4-6 W.m-1·K-1The vanadium dioxide has better heat conduction capability, but the vanadium dioxide is easy to oxidize after being placed in the air for a long time, and the thermal stability is poorer.
Hexagonal boron nitride has a layered crystal structure similar to graphite and is therefore also known as "white graphene". The material has good electrical insulation, thermal conductivity and chemical stability, and is a good fire-resistant and high-temperature-resistant material and a heat-conducting material. Therefore, the vanadium dioxide-boron nitride composite material is expected to be a phase change material with good heat conduction performance and reliable stability.
Disclosure of Invention
In order to solve the background problems, the invention provides a vanadium dioxide-boron nitride phase-change heat-conducting composite material and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
in one aspect, the invention provides a preparation method of a vanadium dioxide-boron nitride phase-change heat-conducting composite material, which comprises the following steps:
carrying out hydrothermal reaction on a vanadium salt, a reducing agent, boron nitride and a doping agent in a solvent;
wherein the boron nitride is hexagonal boron nitride.
In a preferred embodiment, the vanadium salt is a + 5-valent vanadium salt, and specific examples thereof include ammonium metavanadate, ammonium pyrovanadate, ammonium orthovanadate, ammonium polyvanadate, and ammonium decavanadate, and the vanadium salts may be used singly or in any combination thereof.
As a preferred embodiment, the reducing agent is selected from any one or more of oxalic acid, citric acid, formic acid and acetic acid.
As a preferred embodiment, the dopant is selected from any one or more of salts of tungsten, magnesium, molybdenum, niobium, tantalum, zinc, aluminum, copper, transition metal telluride, and oxygen group tellurium compounds;
preferably, the doping agent is selected from any one or a mixture of ammonium tungstate and tellurium dioxide; further preferably, ammonium tungstate and tellurium dioxide are used in combination.
In the technical scheme of the invention, the transition metal telluride can be vanadium telluride, titanium telluride, tungsten telluride, molybdenum telluride, copper telluride, zinc telluride, tin telluride and the like; examples of the tellurium oxogroup compound include tellurium oxide, tellurium sulfide, and tellurium selenide.
As a preferred embodiment, the solvent is an organic solvent, preferably any one or more of ethanol, N-Dimethylformamide (DMF), isopropanol, and N-methylpyrrolidone (NMP).
In a preferred embodiment, the temperature of the hydrothermal reaction is 180 to 260 ℃, for example 180 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 260 ℃ or any value therebetween;
preferably, the time of the hydrothermal reaction is 12-24 h;
preferably, the hydrothermal reaction is carried out under a stirring condition, and the rotation speed of the stirring is preferably 100-500 r/min.
In certain specific embodiments, the method of preparation further comprises post-treatment; the post-treatment comprises centrifuging, washing, drying and annealing; the washing is that ethanol and acetone are respectively washed; the drying is carried out for 4-12 h at the temperature of 40-80 ℃; the annealing is 600-800 ℃ annealing for 2-5 h, such as 600 ℃, 620 ℃, 640 ℃, 660 ℃, 680 ℃, 700 ℃, 720 ℃, 740 ℃, 760 ℃, 780 ℃ and 800 ℃.
In the technical scheme of the invention, the annealing can improve VO with phase change function2Purity of the phase.
As a preferred embodiment, the preparation method specifically comprises the following steps:
1) dissolving ammonium metavanadate, oxalic acid, hexagonal boron nitride, ammonium tungstate and/or tellurium dioxide in a solvent to obtain a dispersion liquid;
2) heating the dispersion liquid obtained in the step 1) to 180-260 ℃ under stirring at a speed of 100-500 r/min, and reacting for 12-24 h;
3) centrifuging the product obtained in the step 2), discarding clear liquid, washing and washing residual reactants by using ethanol and acetone respectively, centrifuging, and drying for 4-12 hours in a vacuum drying oven at the temperature of 40-80 ℃;
4) annealing the product obtained in the step 3) at 600-800 ℃ for 2-5 h to obtain pure-phase-change vanadium dioxide.
Preferably, in the step 1), the usage ratio of ammonium metavanadate, oxalic acid, hexagonal boron nitride, ammonium tungstate and tellurium dioxide is (100-300 mg): (200-700 mg): (50-150 mg): (2.7-7.5 mg): (0.8-4.0 mg).
In another aspect, the invention provides the vanadium dioxide-boron nitride phase-change heat-conducting composite material obtained by the preparation method.
In another aspect, the invention provides an application of the vanadium dioxide-boron nitride phase-change heat-conducting composite material in preparation of a thermal interface material.
The technical scheme has the following advantages or beneficial effects:
according to the invention, a hydrothermal method is adopted to synthesize the vanadium dioxide-boron nitride phase-change heat-conducting composite material, and nano vanadium dioxide is adsorbed on a hexagonal boron nitride nanosheet. In the hydrothermal reaction process, the hexagonal boron nitride powder is hydrothermally stripped into hexagonal boron nitride nanosheets, meanwhile, the pentavalent vanadium source is reduced into tetravalent vanadium, and vanadium dioxide grows on the hexagonal boron nitride nanosheets in situ. On one hand, the vanadium dioxide endows the composite material with phase change heat storage capacity; on the other hand, through the electron-phonon coupling effect between the vanadium dioxide and the boron nitride, higher heat conductivity is obtained under the condition of lower boron nitride loading, the production cost can be reduced, and meanwhile, the boron nitride plays a role in protecting the vanadium dioxide and improves the thermal stability of the vanadium dioxide. Compared with the prior art, the heat conduction oil has the advantages of no oil spilling phenomenon, good thermal stability and high heat conductivity coefficient. In addition, the invention also reduces the phase change temperature of the vanadium dioxide by doping metal ions, and enlarges the application range of the phase change material.
Drawings
Fig. 1 is an SEM image of the vanadium dioxide-boron nitride composite material prepared in example 1.
FIG. 2 is a graph of differential thermal test results for vanadium dioxide-boron nitride composites prepared in examples 1-4 and commercial vanadium dioxide.
FIG. 3 is a Differential Scanning Calorimetry (DSC) curve of the vanadium dioxide-boron nitride composite prepared in example 1 and commercial vanadium dioxide and their heating at 300 ℃ for 3 hours.
Detailed Description
The following examples are only a part of the present invention, and not all of them. Thus, the detailed description of the embodiments of the present invention provided below is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the invention without making creative efforts, belong to the protection scope of the invention.
In the present invention, all the equipment, materials and the like are commercially available or commonly used in the industry, if not specified. The methods in the following examples are conventional in the art unless otherwise specified.
In the following examples, hexagonal boron nitride is in powder form and is available from the national pharmaceutical group chemical agents, ltd.
Example 1:
(1) adding 200mg of ammonium metavanadate, 461.5mg of oxalic acid, 100mg of hexagonal boron nitride and 15mL of isopropanol into a glass beaker, adding 4.36mg of ammonium tungstate and 1.36mg of tellurium dioxide, and stirring for 30min to obtain a dispersion liquid;
(2) transferring the dispersion liquid to a hydrothermal reaction kettle, adding polytetrafluoroethylene stirring magneton, and sealing; under the condition of magnetic stirring, gradually heating the reaction kettle to 260 ℃, setting the stirring speed to be 400r/min, and reacting for 24 hours;
(3) cooling to room temperature after complete reaction, opening the reaction kettle, transferring the product into a centrifuge tube, centrifuging for 10 minutes at 8000 rpm, discarding clear liquid, washing with ethanol and acetone for 1 time respectively, centrifuging again under the same conditions, and drying the product in a vacuum drying oven at 40 ℃ for 5 hours;
(4) and placing the obtained product in a tubular furnace to anneal for 2 hours at 800 ℃ in the nitrogen atmosphere, and cooling to room temperature to obtain the vanadium dioxide-boron nitride phase-change heat-conducting composite material.
The vanadium dioxide-boron nitride phase-change heat-conducting composite material prepared in the embodiment is a nano flaky material, and as shown in fig. 1, vanadium dioxide is successfully attached to a boron nitride nanosheet.
Example 2:
(1) adding 200mg of ammonium metavanadate, 461.5mg of oxalic acid, 100mg of hexagonal boron nitride and 20mL of ethanol into a glass beaker, adding 4.36mg of ammonium tungstate and 2.72mg of tellurium dioxide, and stirring for 30min to obtain a dispersion liquid;
(2) transferring the dispersion liquid into a hydrothermal reaction kettle, adding polytetrafluoroethylene, stirring and sealing; under the condition of magnetic stirring, gradually heating the reaction kettle to 260 ℃, setting the stirring speed to be 400r/min, and reacting for 24 hours;
(3) cooling to room temperature after complete reaction, opening the reaction kettle, transferring the product into a centrifuge tube, centrifuging for 10 minutes at 8000 rpm, discarding clear liquid, washing with ethanol and acetone for 1 time respectively, centrifuging again under the same conditions, and drying the product in a vacuum drying oven at 40 ℃ for 5 hours;
(4) and placing the obtained product in a tubular furnace to anneal for 2 hours at 800 ℃ in the nitrogen atmosphere, and cooling to room temperature to obtain the vanadium dioxide-boron nitride phase-change heat-conducting composite material.
The vanadium dioxide-boron nitride phase-change heat-conducting composite material prepared in the embodiment is a nano flaky material.
Example 3:
(1) adding 200mg of ammonium metavanadate, 461.5mg of oxalic acid, 100mg of hexagonal boron nitride and 20mg of DMF (dimethyl formamide) into a glass beaker, adding 4.36mg of ammonium tungstate, and stirring for 30min to obtain a dispersion liquid;
(2) transferring the dispersion liquid to a hydrothermal reaction kettle, adding polytetrafluoroethylene stirring magneton, and sealing; under the condition of magnetic stirring, gradually heating the reaction kettle to 260 ℃, setting the stirring speed to be 400rpm, and reacting for 24 hours;
(3) cooling to room temperature after complete reaction, opening the reaction kettle, transferring the product into a centrifuge tube, centrifuging for 10 minutes at 8000 rpm, discarding clear liquid, washing with ethanol and acetone for 1 time respectively, centrifuging again under the same conditions, and drying the product in a vacuum drying oven at 40 ℃ for 5 hours;
(4) and placing the obtained product in a tubular furnace to anneal for 2 hours at 800 ℃ in the nitrogen atmosphere, and cooling to room temperature to obtain the vanadium dioxide-boron nitride phase-change heat-conducting composite material.
The vanadium dioxide-boron nitride phase-change heat-conducting composite material prepared in the embodiment is a nano flaky material and has a multi-stage structure.
Example 4:
(1) adding 200mg of ammonium metavanadate, 461.5mg of oxalic acid, 100mg of hexagonal boron nitride and 20mg of NMP into a glass beaker, adding 2.72mg of tellurium dioxide, and stirring for 0.5 hour to obtain a dispersion liquid;
(2) transferring the dispersion liquid to a hydrothermal reaction kettle, adding polytetrafluoroethylene stirring magneton, and sealing; under the condition of magnetic stirring, gradually heating the reaction kettle to 260 ℃, setting the stirring speed to be 400r/min, and reacting for 24 hours;
(3) cooling to room temperature after complete reaction, opening the reaction kettle, transferring the product into a centrifuge tube, centrifuging for 10 minutes at 8000/min, discarding clear liquid, washing with ethanol and acetone for 1 time respectively, centrifuging again under the same conditions, and drying the product in a vacuum drying oven at 40 ℃ for 5 hours;
(4) and placing the obtained product in a tube furnace to anneal for 2 hours at 800 ℃ under the nitrogen atmosphere, and cooling to room temperature to obtain the vanadium dioxide-boron nitride phase-change heat-conducting composite material.
The vanadium dioxide-boron nitride phase-change heat-conducting composite material prepared in the embodiment is a nano flaky material.
Effects of the embodiment
(1) And (3) testing thermal conductivity:
the vanadium dioxide-boron nitride phase-change thermal-conductive composite materials prepared in examples 1-4 were added to bisphenol a epoxy resin (containing 40 wt% of curing agent) at 40 wt%, stirred and defoamed in a vacuum blender at 2000r/min for 30min, poured into a mold, cured at 165 ℃ for 2h to obtain test sample blocks, and tested for thermal conductivity on a hot wire transient thermal conductivity instrument, with the test results shown in table 1.
TABLE 1
As can be seen from Table 1, the composite material prepared by the present invention has good thermal conductivity, wherein when tungsten and tellurium are doped simultaneously, the composite material has better thermal conductivity.
(2) Differential scanning calorimetry test:
fig. 2 shows the differential calorimetric test results of the composite materials of examples 1-4 of the present invention and commercial pure vanadium dioxide, and it can be seen from the graph that the composite materials of examples 1-4 of the present invention maintain the first-order phase transition characteristic of vanadium dioxide, and have lower phase transition temperature than commercial pure vanadium dioxide.
(3) Thermal stability:
FIG. 3 shows commercially pure vanadium dioxide (VO)2) And vanadium dioxide-boron nitride (VO) prepared in inventive example 12-BN) composite material and a Differential Scanning Calorimetry (DSC) curve thereof after heating for 3h at 300 ℃. As can be seen from the figure, pure VO2After the heating oxidation treatment, the DSC peak is obviously weakened, namely the thermal stability is poor; and VO2The DSC peak of the-BN composite material is not obviously changed before and after the heating oxidation treatment, which shows that the thermal stability of the-BN composite material is obviously improved.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention, and such modifications and adaptations are intended to be within the scope of the invention.
Claims (10)
1. The preparation method of the vanadium dioxide-boron nitride phase-change heat-conducting composite material is characterized by comprising the following steps of:
carrying out hydrothermal reaction on a vanadium salt, a reducing agent, boron nitride and a doping agent in a solvent;
wherein the boron nitride is hexagonal boron nitride.
2. The method according to claim 1, wherein the vanadium salt is a + 5-valent vanadium salt.
3. The method according to claim 1, wherein the reducing agent is selected from any one or more of oxalic acid, citric acid, formic acid and acetic acid.
4. The preparation method according to claim 1, wherein the dopant is selected from any one or more of (i) salts of tungsten, magnesium, molybdenum, niobium, tantalum, zinc, aluminum, copper, (ii) transition metal telluride, and (iii) chalcogen tellurium compounds;
preferably, the doping agent is selected from any one or a mixture of ammonium tungstate and tellurium dioxide; further preferably, ammonium tungstate and tellurium dioxide are used in combination.
5. The method according to claim 1, wherein the solvent is an organic solvent, preferably one or more selected from the group consisting of ethanol, N-dimethylformamide, isopropanol, and N-methylpyrrolidone.
6. The preparation method according to claim 1, wherein the temperature of the hydrothermal reaction is 180-260 ℃;
preferably, the time of the hydrothermal reaction is 12-24 h;
preferably, the hydrothermal reaction is carried out under a stirring condition, and the rotation speed of the stirring is preferably 100-500 r/min.
7. The method of claim 1, further comprising post-processing; the post-treatment comprises centrifuging, washing, drying and annealing; the washing is that ethanol and acetone are respectively washed; the drying is carried out for 4-12 h at the temperature of 40-80 ℃; the annealing is carried out at the temperature of 600-800 ℃ for 2-5 h.
8. The preparation method according to claim 1, comprising in particular the steps of:
1) dissolving ammonium metavanadate, oxalic acid, hexagonal boron nitride, ammonium tungstate and/or tellurium dioxide in a solvent to obtain a dispersion liquid;
2) heating the dispersion liquid obtained in the step 1) to 180-260 ℃ under stirring at a speed of 100-500 r/min, and reacting for 12-24 h;
3) centrifuging the product obtained in the step 2), discarding clear liquid, washing and washing residual reactants by using ethanol and acetone respectively, centrifuging, and drying for 4-12 hours in a vacuum drying oven at the temperature of 40-80 ℃;
4) annealing the product obtained in the step 3) at 600-800 ℃ for 2-5 h to obtain pure-phase-change vanadium dioxide;
preferably, in the step 1), the usage ratio of ammonium metavanadate, oxalic acid, hexagonal boron nitride, ammonium tungstate and tellurium dioxide is (100-300 mg): (200-700 mg): (50-150 mg): (2.7-7.5 mg): (0.8-4.0 mg).
9. The vanadium dioxide-boron nitride phase-change heat-conducting composite material prepared by the preparation method of any one of claims 1-8.
10. Use of the vanadium dioxide-boron nitride phase change thermal conductive composite material of claim 9 in the preparation of a thermal interface material.
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