CN114292628A - Bamboo-like phase-change heat storage material and preparation method thereof - Google Patents
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Abstract
The invention discloses a bamboo-like phase change heat storage material and a preparation method thereof, wherein molten silicon reacts with a carbonized bamboo structure to generate porous silicon carbide ceramic in a bamboo shape, and inorganic salt is immersed into a silicon carbide framework in vacuum to obtain a composite material with high heat conductivity (35W/m.K) and high energy storage density (309 kJ/kg). In addition, titanium nitride is loaded on the surface of the silicon carbide, and the composite photo-thermal storage material is obtained after the titanium nitride is immersed in paraffin in vacuum, and the spectral absorption is up to 96%. The high heat conduction and high spectral absorptivity of bamboo derived silicon carbide enable the intensity of incident light to be 1.62W/cm2In time, the photothermal storage efficiency of the composite material reaches 91.1%. The bamboo derived silicon carbide ceramic has continuous heat transport channels and extremely high spectral absorption rate, so that high heat conduction, high energy storage density and high light-heat conversion efficiency can be realized simultaneously. The invention provides more possibilities for bamboo derived silicon carbide ceramics in the aspects of excellent photothermal conversion and storage.
Description
Technical Field
The invention belongs to the technical field of phase change energy storage material preparation, and particularly relates to a bamboo-derived silicon carbide ceramic photo-thermal storage material with phase change heat storage and a preparation method thereof.
Background
With the rapid development of social economy, the traditional fossil fuel is rapidly consumed, and a series of environmental problems are caused. Solar energy is the cleanest and most abundant renewable energy source and has received extensive attention from researchers. Among the various forms of solar energy utilization, solar thermal conversion is considered a promising approach because of its ability to collect full spectrum solar energy and high efficiency. However, the practical application of the technology is limited by the inherent shortcomings of the solar energy such as time-break and seasonal influence. To overcome these drawbacks, thermal energy storage was introduced to bridge the gap between fluctuating energy supply and continuous energy demand.
The heat storage technology mainly comprises sensible heat storage, thermochemical heat storage and phase change heat storage. Compared with the other two heat storage technologies, the phase change material has larger energy storage capacity, smaller temperature change and better chemical stability in latent heat storage. Solar heat conversion and latent heat storage are integrated, namely, the phase change material is used for directly absorbing solar energy, and the latent heat storage process is driven through the phase change process, so that the solar heat storage device is a new technology for effectively improving instability and unbalance of supply and demand of solar energy. Phase change materials generally have lower thermal conductivity and lower spectral absorption. Conventional high thermal conductivity materials are realized by filling high thermal conductivity inorganic fillers such as aluminum nitride particles, metal particles, graphene, and the like. However, the increase in filler content is accompanied by a high cost, a high weight and impairment of the mechanical properties of the material. It is currently difficult to achieve high thermal conductivity at low loading levels by simply blending. In the case of simple blending, the composite material is difficult to form a heat path and has larger heat transfer resistance. And the metal material is easy to corrode, and the carbon-based material is easy to corrode at high temperature. Compared with metal materials and carbon-based materials, the silicon carbide has good physical and chemical stability and higher thermal conductivity.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method of bamboo-derived silicon carbide ceramic, titanium nitride and paraffin photo-thermal heat storage material for phase change heat storage, a bamboo-derived silicon carbide ceramic composite storage material and a preparation method thereof.
The technical scheme is as follows: the bamboo-derived silicon carbide ceramic photo-thermal storage material with phase change heat storage is prepared by compounding paraffin, titanium nitride and a silicon carbide porous framework; or the storage material is prepared by compounding lithium hydroxide, lithium fluoride and a silicon carbide porous framework.
Further, the titanium nitride is nano-particles, and the particle size is 40-60 nm.
Further, the silicon carbide porous skeleton is coated in the eutectic salt material.
The invention discloses a preparation method of a bamboo derived silicon carbide ceramic photothermal storage material with phase change heat storage, which comprises the following steps:
(1) after the bamboo is primarily cut, putting the bamboo into an oven for drying for 3-4 days, putting the bamboo into a tube furnace, and preserving heat for 0.5h at the inert atmosphere temperature of 900 ℃ to obtain carbonized bamboo; further cutting the carbonized sample, and preserving heat for 1.5-2h at 1600 ℃ in a vacuum environment for silicon melting reaction under the condition of excessive silicon powder; then heating to 1800 ℃ at a heating rate of 15 ℃/min to perform a silicon removal reaction, and repeating for multiple times to ensure that the excessive silicon is completely removed;
(2) dispersing titanium nitride in alcohol, and performing ultrasonic treatment to obtain a mixed solution; immersing the silicon carbide framework into the mixed solution, repeatedly immersing, drying in an oven, and sintering in a muffle furnace to obtain a silicon carbide-titanium nitride composite framework;
(3) and putting the obtained composite framework into paraffin, placing the paraffin in a vacuum oven, and immersing the paraffin in the vacuum oven at the temperature of 80-90 ℃ to obtain the composite photo-thermal storage material.
Further, in the step (1), the temperature is raised to 500 ℃ at the heating rate of 0.5 ℃/min under the inert atmosphere, then raised to 900 ℃ at the heating rate of 1 ℃/min, and the temperature is maintained for 0.5 h.
Further, the method is characterized in that in the step (1), the mass ratio of the silicon powder to the bamboo charcoal is 3.5-4: 1.
Further, the method is characterized in that in the step (2), titanium nitride is dispersed in alcohol with the mass ratio of 1:99, and ultrasonic treatment is carried out for 1 hour to obtain a mixed solution; and (3) immersing the silicon carbide framework into the mixed solution, repeatedly immersing, putting into an oven, drying at 150 ℃ for 24h, and putting into a muffle furnace, and keeping the temperature at 300 ℃ for 1h to obtain the composite framework.
The invention discloses another preparation method of a bamboo-derived silicon carbide ceramic photothermal storage material with phase change heat storage, which comprises the following steps:
(1) and after the bamboo is primarily cut, putting the bamboo into an oven for drying for 3-4 days, putting the bamboo into a tube furnace, preserving heat for 0.5h at the inert atmosphere temperature of 900 ℃ to obtain carbonized bamboo, further cutting the carbonized sample, and preserving heat for 1.5-2h at 1600 ℃ in a vacuum environment under the condition of excessive silicon powder for silicon melting reaction. Then heating to 1800 ℃ at a heating rate of 15 ℃/min to perform a silicon removal reaction, and repeating for multiple times to ensure that the excessive silicon is completely removed;
(2) fully mixing lithium hydroxide and lithium fluoride in a planetary ball mill, fully drying and storing for later use;
(3) and putting the eutectic salt and the porous silicon carbide framework into a graphite crucible and placing the graphite crucible and the porous silicon carbide framework into a tubular furnace, heating to 500 ℃ in a vacuum atmosphere, and preserving heat for 3-4 hours to obtain the composite heat storage material.
Further, in the step (2), the lithium hydroxide and the lithium fluoride are mixed in a planetary ball mill at a molar ratio of LiOH to LiF of 80:20 mol.% for 3-4h at a rotation speed of 300rpm, and are dried at 100 ℃ for 24h under an inert atmosphere, and then dried at 350 ℃ for 1h, so as to obtain the heat storage material.
Further, the porous silicon carbide framework is coated on eutectic salt and placed in a graphite crucible to be placed in a tube furnace, the temperature is raised to 500 ℃ in a vacuum atmosphere, and heat preservation is carried out for 3 hours, so that the composite heat storage material is obtained.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: according to the bamboo-derived silicon carbide ceramic, a three-dimensional silicon carbide network is constructed, a continuous high-heat-conduction channel is formed, and the heat conductivity of the phase-change material is effectively improved under the condition of low load capacity. By adopting bamboo as a porous structure template, porous SiC ceramics with different porosities (66% -77%) are prepared, and a continuous channel structure with orderly arranged bamboo is copied. The biological form SiC ceramic composite material embedded with LiOH/LiF eutectic can simultaneously realize high heat conduction of 35W/m.K and high energy storage density of 309 kJ/kg. In addition, after titanium nitride is loaded on the surface of the silicon carbide framework, the silicon carbide framework is compounded with the phase-change material. The ultrahigh energy storage efficiency is obtained by utilizing the high absorption rate and the high heat conduction performance of the composite material. The illumination intensity is 1.62W/cm2And the energy storage efficiency can reach 91.1%. Thus, bamboo-derived silicon carbide ceramics can be realized simultaneouslyRapid heat storage, large energy storage density and high solar energy storage efficiency.
Drawings
FIG. 1 is a schematic diagram of the present invention;
FIG. 2 is an SEM image of carbonized bamboo;
FIG. 3 is an SEM image of bamboo-like silicon carbide;
FIG. 4 is a graph of the thermal conductivity of silicon carbide and paraffin composites at different porosities;
FIG. 5 is the latent heat of phase change of the composite material;
FIG. 6 is the spectral absorption of the composite;
fig. 7 shows the photo-thermal storage efficiency at different illumination intensities.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
The method for measuring each parameter in the implementation and proportion of the invention is
1. And measuring the thermal conductivity of the material by using a laser thermal conductivity meter.
2. The material was tested for latent heat of phase change using DSC (differential scanning calorimetry).
3. The spectral absorptance of the material was measured using a spectrophotometer.
4. Measuring radiation intensity under different illumination by using power meter
Embodiments of the invention are further illustrated by the following examples:
fully drying the bamboo, and carbonizing to obtain the carbon template. And fully reacting the obtained carbon template with excessive silicon powder to obtain the silicon carbide porous structure. The composite material is obtained after the phase-change material is immersed under vacuum, and the basic principle is shown in figure 1. The bamboo derived silicon carbide ceramic photo-thermal storage material mainly comprises the following implementation modes:
the first step is as follows: preparation of bamboo-derived silicon carbide ceramic
Firstly, simply cutting the bamboo, cutting the bamboo into sections, and then putting the bamboo into an oven to dry the bamboo for three days at 70 ℃. After fully drying, heating to 500 ℃ at the heating rate of 0.5 ℃/min, heating to 900 ℃ at the heating rate of 1 ℃/min, and keeping the temperature for half an hour under the argon atmosphere to obtain a carbonized bamboo structure, wherein an SEM image of the carbon template is shown in figure 2. The carbonized sample was cut into a cylindrical sample having a thickness of 4mm and a diameter of 15 mm. And keeping the temperature of 1600 ℃ for 1.5h in a vacuum atmosphere at the mass ratio of silicon to carbon of 3.5 to carry out siliconizing reaction, thus obtaining a composite sample of silicon and silicon carbide. And raising the temperature of the composite sample to 1800 ℃ at a heating rate of 15 ℃/min to perform silicon removal reaction, and repeating the reaction for multiple times to ensure that the excessive silicon is completely removed. The morphology of the resulting silicon carbide after removal of the excess silicon is shown in figure 3. The obtained silicon carbide ceramic was further cut to obtain a cylindrical sample having a diameter of 13mm and a thickness of 3mm for subsequent processing.
The second step is that: preparation of silicon carbide-titanium nitride composite framework
0.05g of titanium nitride and 0.495g of alcohol were mixed together, and after one hour of ultrasonic treatment, a mixed solution was obtained. And (3) immersing the silicon carbide framework into the mixed solution, repeatedly immersing, putting into an oven, drying at 150 ℃ for 24h, and putting into a muffle furnace, and keeping the temperature at 300 ℃ for 1h to obtain the composite framework.
The third step: preparation of photothermal storage material
And (3) embedding the composite framework obtained in the first step into excessive paraffin, putting the composite framework into a vacuum oven, and preserving heat for 2 hours at 80 ℃ to obtain the photo-thermal storage material.
The preparation method of the bamboo derived silicon carbide ceramic composite heat storage material comprises the following steps:
the first step is as follows: preparation of bamboo-derived silicon carbide ceramic
Firstly, simply cutting the bamboo, cutting the bamboo into sections, and then putting the bamboo into an oven to dry the bamboo for three days at 70 ℃. After full drying, heating to 500 ℃ at the heating rate of 0.5 ℃/min, then heating to 900 ℃ at the heating rate of 1 ℃/min, and preserving heat for half an hour under the argon atmosphere to obtain the carbonized bamboo structure. The carbonized sample was cut into a cylindrical sample having a thickness of 4mm and a diameter of 15 mm. And keeping the temperature of 1600 ℃ for 1.5h in a vacuum atmosphere at the mass ratio of silicon to carbon of 3.5 to carry out siliconizing reaction, thus obtaining a composite sample of silicon and silicon carbide. And raising the temperature of the composite sample to 1800 ℃ at a heating rate of 15 ℃/min to perform silicon removal reaction, and repeating the reaction for multiple times to ensure that the excessive silicon is completely removed. The obtained silicon carbide ceramic was further cut to obtain a cylindrical sample having a diameter of 13mm and a thickness of 3mm for subsequent processing.
The second step is that: preparation of medium-temperature phase-change material
The molar ratio of lithium hydroxide to lithium fluoride was LiOH: LiF 80:20 mol.%, the mass of lithium hydroxide was 7.9g, and the mass of lithium fluoride was 2.1 g. And mixing the lithium hydroxide and the lithium fluoride in a planetary ball mill at the rotating speed of 300rpm for three hours, drying at 100 ℃ for 24 hours under an inert atmosphere, and drying at 300 ℃ for 1 hour to obtain the intermediate-temperature phase-change material for subsequent use.
The third step: preparation of medium-temperature composite storage material
And embedding the prepared silicon carbide framework into an excessive phase-change material, and putting the silicon carbide framework into a tubular furnace to preserve heat for 3 hours at 500 ℃ in a vacuum atmosphere to obtain the intermediate-temperature composite heat storage material.
The performance parameters of the bamboo-derived silicon carbide photo-thermal storage material and the composite heat storage material prepared by the implementation are as follows:
after the silicon carbide and the eutectic salt are compounded, the thermal conductivity can reach 35W/m.K, and the energy storage density can reach 309kJ/kg from figure 5. After the silicon carbide surface is loaded with the titanium nitride, the average spectral absorption of the composite material obtained from fig. 6 can reach 96.23%, which shows that the titanium nitride can effectively improve the spectral absorption capacity of the composite material. As shown in FIG. 7, the intensity of light irradiation was 1.62W/cm2In time, the composite material has high heat conduction and high spectral absorption performance, so that the photo-thermal energy storage efficiency can reach 91.1%. The thermal conductivity of bamboo-derived silicon carbide ceramics of different porosities is as high as 40W/m.K at a porosity of 66%, as shown in FIG. 4.
Claims (10)
1. A bamboo-like phase change heat storage material is characterized in that the storage material is prepared by compounding paraffin, titanium nitride and a silicon carbide porous skeleton; or the storage material is prepared by compounding lithium hydroxide, lithium fluoride and a silicon carbide porous framework.
2. The bamboo-like phase change heat storage material as claimed in claim 1, wherein the titanium nitride is in the form of nanoparticles with a particle size of 40-60 nm.
3. The bamboo-like phase change heat storage material as claimed in claim 1, wherein the porous framework of silicon carbide is encapsulated in eutectic salt material.
4. A method for preparing the bamboo-like phase change heat storage material of claim 1, comprising the following steps:
(1) after the bamboo is primarily cut, putting the bamboo into an oven for drying for 3-4 days, putting the bamboo into a tube furnace, and preserving heat for 0.5h at the inert atmosphere temperature of 900 ℃ to obtain carbonized bamboo; further cutting the carbonized sample, and preserving heat for 1.5-2h at 1600 ℃ in a vacuum environment for silicon melting reaction under the condition of excessive silicon powder; then heating to 1800 ℃ at a heating rate of 15 ℃/min to perform a silicon removal reaction, and repeating for multiple times to ensure that the excessive silicon is completely removed;
(2) dispersing titanium nitride in alcohol, and performing ultrasonic treatment to obtain a mixed solution; immersing the silicon carbide framework into the mixed solution, repeatedly immersing, drying in an oven, and sintering in a muffle furnace to obtain a silicon carbide-titanium nitride composite framework;
(3) and putting the obtained composite framework into paraffin, placing the paraffin in a vacuum oven, and immersing the paraffin in the vacuum oven at the temperature of 80-90 ℃ to obtain the composite photo-thermal storage material.
5. The method for preparing a bamboo-like phase change heat storage material as claimed in claim 4, wherein in the step (1), the temperature is raised to 500 ℃ at a heating rate of 0.5 ℃/min, then raised to 900 ℃ at a heating rate of 1 ℃/min, and the temperature is maintained for 0.5h under an inert atmosphere.
6. The preparation method of the bamboo-like phase change heat storage material as claimed in claim 4, wherein in the step (1), the mass ratio of the silicon powder to the bamboo charcoal during the silicon melting reaction is 3.5-4: 1.
7. the preparation method of the bamboo-like phase change heat storage material according to claim 4, wherein in the step (2), titanium nitride is dispersed in alcohol in a mass ratio of 1:99, and ultrasonic treatment is performed for 1 hour to obtain a mixed solution; and (3) immersing the silicon carbide framework into the mixed solution, repeatedly immersing, putting into an oven, drying at 150 ℃ for 24h, and putting into a muffle furnace, and keeping the temperature at 300 ℃ for 1h to obtain the composite framework.
8. A method for preparing the bamboo-like phase change heat storage material of claim 1, comprising the following steps:
(1) and after the bamboo is primarily cut, putting the bamboo into an oven for drying for 3-4 days, putting the bamboo into a tube furnace, preserving heat for 0.5h at the inert atmosphere temperature of 900 ℃ to obtain carbonized bamboo, further cutting the carbonized sample, and preserving heat for 1.5-2h at 1600 ℃ in a vacuum environment under the condition of excessive silicon powder for silicon melting reaction. Then heating to 1800 ℃ at a heating rate of 15 ℃/min to perform a silicon removal reaction, and repeating for multiple times to ensure that the excessive silicon is completely removed;
(2) fully mixing lithium hydroxide and lithium fluoride in a planetary ball mill, fully drying and storing for later use;
(3) and putting the eutectic salt and the porous silicon carbide framework into a graphite crucible and placing the graphite crucible and the porous silicon carbide framework into a tubular furnace, heating to 500 ℃ in a vacuum atmosphere, and preserving heat for 3-4 hours to obtain the composite heat storage material.
9. The preparation method of the bamboo-like phase change heat storage material according to claim 8, wherein in the step (2), the lithium hydroxide and the lithium fluoride are mixed in a planetary ball mill at a molar ratio of LiOH to LiF of 80:20 mol.% for 3-4h at a rotation speed of 300rpm, and are dried at 100 ℃ for 24h under an inert atmosphere, and then are dried at 350 ℃ for 1h to obtain the heat storage material.
10. The preparation method of the bamboo-like phase change heat storage material as claimed in claim 8, wherein the porous silicon carbide skeleton is coated on eutectic salt, placed in a graphite crucible and placed in a tube furnace, and heated to 500 ℃ in a vacuum atmosphere and insulated for 3 hours to obtain the composite heat storage material.
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Application publication date: 20220408 |