CN112592695A - Shell-like structure bionic composite phase-change heat storage material and preparation method thereof - Google Patents
Shell-like structure bionic composite phase-change heat storage material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a shell-like structure bionic composite phase-change heat storage material and a preparation method thereof, wherein the shell-like structure bionic composite phase-change heat storage material comprises a phase-change material, a sheet-shaped porous structure ceramic framework and a ceramic additive; wherein the porosity of the ceramic framework with the sheet-shaped pore structure is 50-85%, and the mass percentage of the ceramic additive is 0-10%. The heat conductivity coefficient of the phase change heat storage material can be greatly improved. The invention forms the compound of the shell-like structure by immersing the phase-change material in the high-heat conductivity coefficient ceramic skeleton with the sheet-shaped pore structure prepared by the freeze-drying method under the vacuum condition. The method has the advantages of simple preparation process and high adjustability, and the prepared composite material can be used in the fields of solar building heating, waste heat utilization and the like.
Description
Technical Field
The invention relates to the technical field of heat storage materials produced by chemical and chemical methods and the field of energy material science, in particular to a shell-like structure bionic composite phase-change heat storage material and a preparation method thereof.
Background
With the further consumption of energy resources and the further implementation of the reform policy on the energy supply side in China, the research trend of how to efficiently utilize solar energy and waste heat generated by the industry becomes. The phase-change heat storage technology does not involve chemical changes, and the temperature is kept unchanged while a large amount of heat is stored by utilizing the phase-change process in the using process. However, the low thermal conductivity of the phase-change heat storage material is a major disadvantage, and limits the effectiveness of the phase-change heat storage material in practical situations of solar energy or waste heat utilization.
At present, for phase change heat storage materials, heat conductivity coefficient is improved by a common method, and most practical measures are to add high heat conduction particles or traditional metal or ceramic frameworks in the phase change materials. Many biological structures in nature have excellent performance, which is more worth being used for reference, but at present, the preparation of the high-thermal-conductivity ceramic skeleton in the bionic field is rarely researched.
Therefore, in order to improve the heat conductivity coefficient of the phase change material, the invention provides a method for preparing the composite phase change material with the shell-like structure by taking the shell surface architecture in the sea as a reference, so as to improve the heat conductivity coefficient.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a bionic composite phase-change material with high adjustability, low cost and high efficiency and a preparation method thereof, wherein the bionic composite phase-change material has higher heat conductivity coefficient and is beneficial to a shell-like bionic structure, so that the composite phase-change material has the advantages of high heat storage density, high heat conductivity coefficient and high structural strength.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
the invention provides a shell-like structure bionic phase-change heat storage material which is characterized by comprising a sheet-shaped pore structure ceramic framework, a ceramic additive and a phase-change material soaked in pores of the ceramic framework, wherein the porosity of the sheet-shaped pore structure ceramic framework is 50-85%, the mass percentage of the ceramic additive is 0-10%, and the ceramic framework accounts for 15-50% of the composite phase-change heat storage material by volume percentage;
the phase-change material is one or more than two of organic phase-change material sugar alcohols and inorganic phase-change material inorganic salts; the ceramic framework is made of SiC, AlN, Al2O3, MgO, TiN, SiO2 and the like as matrix materials; the ceramic additive is one or a plurality of combination modes of yttrium oxide, aluminum oxide, lanthanum oxide, sodium carboxymethylcellulose, polyvinyl alcohol and sodium dodecyl benzene sulfonate.
The phase-change heat storage material is 1 or more than 2 of lipid, sugar alcohol such as erythritol, mannitol, paraffin and the like, nitrate, carbonate and chloride salt such as lithium nitrate, sodium chloride, lithium carbonate and the like. Erythritol and lithium nitrate are particularly preferred.
The ceramic framework is one or a combination of at least two of SiC, AlN, Al2O3, MgO, TiN and SiO2, and more preferably 1 or 2 of SiC, AlN and Al2O 3.
The ceramic additive is one or more of yttrium oxide, aluminum oxide, lanthanum oxide, sodium carboxymethylcellulose, polyvinyl alcohol and sodium dodecyl benzene sulfonate, and is preferably 1 or 2 of yttrium oxide, aluminum oxide, sodium carboxymethylcellulose and sodium dodecyl benzene sulfonate.
The freeze drying prefreezing temperature is-90 to-20 ℃, the bottom of the mold is a metal bottom plate with high thermal conductivity coefficient, preferably a copper sheet, the periphery of the side surface is made of a material with low thermal conductivity coefficient, preferably polytetrafluoroethylene or PMMA, and the top of the mold is open.
The sintering inert atmosphere is nitrogen or argon, and the sintering temperature is 1400-2050 ℃.
A preparation method of a shell-like structure bionic composite phase-change heat storage material comprises the following steps:
step 3, discharging the ceramic additives from the ceramic blank in the step 2 at a low temperature, and sintering the ceramic blank in a high-temperature furnace in an inert atmosphere without pressure;
and 6, taking out the sample, and polishing and grinding the surface to obtain the bionic composite phase-change heat storage material with the shell-like structure.
Compared with the prior art, the invention has the following remarkable advantages:
the invention utilizes the freeze drying technology to prepare the ceramic framework with multilayer flaky holes, and then utilizes the capillary adsorption effect of the porous framework to fill the molten phase change material in the flaky hole interlayer, thereby forming the composite phase change material with the shell-like interlayer structure, wherein the inorganic mineral layer on the surface of the shell corresponds to the ceramic framework, the organic protein layer corresponds to the phase change heat storage material, the ceramic framework has higher heat conductivity coefficient, and is beneficial to the bionic structure of the shell-like shell, so that the composite phase change material has the advantages of large heat storage density, high heat conductivity coefficient and high structural strength, and has better application prospect in the fields of solar energy utilization, building heating, industrial waste heat utilization and the like. Its advantage is: the highly ordered ceramic skeleton in the compound with the shell-like structure (1) serves as a good heat conduction channel, so that the heat conduction coefficient is large, and heat can be rapidly stored. (2) The shell-like structure of the composite has sandwich structure properties, so that the mechanical strength thereof is enhanced. (3) The preparation method is simple, the cost is low, the adjustability is wide, the adjustability can be achieved according to various application scenes, and the composite material is non-toxic and pollution-free.
Drawings
FIG. 1 is a SEM image of the skeleton of a sheet-like porous structure of example 1;
FIG. 2a is a SEM image of the skeleton of a lamellar pore structure according to example 3;
FIG. 2b is an SEM image of a composite phase change material of example 3;
FIG. 2c is a DSC plot of the composite phase change material of example 3;
FIG. 2d is the laser thermal conductivity test curve of the composite phase change material of example 3, with a measured thermal diffusivity of 0.195cm2The calculated corresponding thermal conductivity of the/s input density and specific heat should be 25.64W/m K;
FIG. 3 is a graph comparing the thermal conductivity of silicon carbide backbones at different solids levels for example 5.
Detailed Description
Example 1
Uniformly mixing 20g of silicon carbide powder, 0.2g of yttrium oxide, 0.2g of aluminum oxide and 0.2g of sodium carboxymethylcellulose, adding 19.26g of deionized water to ensure that the solid contents are respectively 20vol%, 25vol%, 27.5vol% and 30vol%, then transferring the mixture into a ball milling tank to perform ball milling for 2 hours at the rotating speed of 300r/min, putting the milled ceramic slurry into a vacuum drying box to perform degassing for 10 minutes, then pouring the ceramic slurry into a mould, putting the mould into a freeze dryer, and performing vacuum drying after pre-freezing for 1 hour at the temperature of minus 40 ℃. After the freeze drying is finished, the ceramic biscuit after freeze drying is subjected to air firing in a muffle furnace at 500 ℃ for 4 hours to remove the sodium carboxymethyl cellulose, and then is subjected to air firing in a hot pressing furnace at 1950 ℃ for 4 hours to obtain the silicon carbide ceramic skeleton with the sheet-mounted oriented pore structure. And (2) putting 20g of erythritol into a 150 ℃ oven for melting, transferring into a 130 ℃ vacuum environment, putting the sintered silicon carbide ceramic skeleton into the molten composite phase-change material, and infiltrating for 2 hours in vacuum. And grinding and polishing the blank into a regular shape after finishing. Fig. 1 is an SEM image of the porous silicon carbide ceramic having a sheet-like pore structure according to the present embodiment.
Example 2
20g of surface-modified aluminum nitride powder, 0.4g of yttrium oxide and 0.2g of carboxymethyl cellulose
And after sodium is uniformly mixed, adding 19.26g of deionized water to ensure that the solid content is respectively 20vol%, 25vol%, 27.5vol% and 30vol%, then transferring the mixture into a ball milling tank to perform ball milling for 2h at the rotating speed of 300r/min, putting the milled ceramic slurry into a vacuum drying oven to degas for 10min, then pouring the degassed ceramic slurry into a mold, putting the mold into a freeze dryer, performing vacuum drying and freeze drying after pre-freezing for 1h at-40 ℃, then performing air firing on the freeze-dried ceramic biscuit for 4h in a muffle furnace at 500 ℃ to remove sodium carboxymethyl cellulose, and then performing non-pressure sintering for 4h at 1900 ℃ in a hot pressing furnace to obtain the silicon carbide ceramic skeleton with the plate-mounted directional hole structure. And (2) putting 20g of lithium nitrate into a furnace at 270 ℃ for melting, then transferring into a vacuum environment at 260 ℃, putting the sintered silicon carbide ceramic skeleton into the molten composite phase-change material, and infiltrating for 1 hour in vacuum. And grinding and polishing the blank into a regular shape after finishing.
Example 3
Uniformly mixing 20g of silicon carbide powder, 0.4g of yttrium oxide, 0.4g of alumina, 0.2g of sodium carboxymethylcellulose and 0.1g of sodium dodecyl benzene sulfonate, adding 16.77g of deionized water to ensure that the solid contents are respectively 20vol%, 25vol%, 27.5vol% and 30vol%, then transferring the mixture into a ball milling tank to perform ball milling for 2 hours at the rotating speed of 600r/min, putting the milled ceramic slurry into a vacuum drying box to perform degassing for 10 minutes, then pouring the ceramic slurry into a mold, putting the ceramic slurry into a freeze dryer, and performing vacuum drying after pre-freezing for 1 hour at the temperature of minus 40 ℃. After the freeze drying is finished, the ceramic biscuit after freeze drying is subjected to air firing in a muffle furnace at 500 ℃ for 4 hours to remove sodium carboxymethyl cellulose and sodium dodecyl benzene sulfonate, and then is subjected to pressureless sintering in a hot pressing furnace at 1950 ℃ for 4 hours to obtain the silicon carbide ceramic skeleton with the sheet-mounted oriented pore structure. And (2) putting 20g of erythritol into a 150 ℃ oven for melting, then transferring into a 130 ℃ vacuum environment, putting the sintered silicon carbide ceramic skeleton into the molten composite phase-change material, and infiltrating for 2 hours in vacuum. And grinding and polishing the blank into a regular shape after finishing. Fig. 2a is an SEM image of the porous silicon carbide ceramic with a lamellar pore structure in the present embodiment, fig. 2b is an SEM image of the shell-like structure composite phase change material in the present embodiment, and fig. 2c is a DSC graph of the shell-like structure composite phase change material in the present embodiment
Example 4
Uniformly mixing 20g of silicon carbide powder, 0.2g of yttrium oxide, 0.2g of aluminum oxide and 0.1g of polyvinyl alcohol, adding 19.26g of deionized water to ensure that the solid contents are respectively 20vol%, 25vol%, 27.5vol% and 30vol%, then transferring the mixture into a ball milling tank to perform ball milling for 2 hours at the rotating speed of 600r/min, putting the milled ceramic slurry into a vacuum drying box to perform degassing for 10 minutes, then pouring the ceramic slurry into a mold, putting the ceramic slurry into a freeze dryer, and performing vacuum drying after pre-freezing for 1 hour at the temperature of minus 40 ℃. After the freeze drying is finished, the ceramic biscuit after freeze drying is subjected to air firing in a muffle furnace at 500 ℃ for 4 hours to remove polyvinyl alcohol, and then is subjected to air firing in a hot pressing furnace at 1950 ℃ for 4 hours to obtain the silicon carbide ceramic skeleton with the sheet-mounted oriented pore structure. And (2) putting 20g of erythritol into a 150 ℃ oven for melting, then transferring into a 130 ℃ vacuum environment, putting the sintered silicon carbide ceramic skeleton into the molten composite phase-change material, and infiltrating for 2 hours in vacuum. And grinding and polishing the blank into a regular shape after finishing.
Example 5
Uniformly mixing 20g of silicon carbide powder, 0.3g of yttrium oxide, 0.3g of aluminum oxide and 0.2g of sodium carboxymethylcellulose, adding 19.26g of deionized water to ensure that the solid contents are respectively 20vol%, 25vol%, 27.5vol% and 30vol%, then transferring the mixture into a ball milling tank to perform ball milling for 2 hours at the rotating speed of 600r/min, putting the milled ceramic slurry into a vacuum drying box to perform degassing for 10 minutes, then pouring the ceramic slurry into a mold, putting the ceramic slurry into a freeze dryer, and performing vacuum drying after pre-freezing for 1 hour at the temperature of minus 40 ℃. After the freeze drying is finished, the ceramic biscuit after freeze drying is subjected to air firing in a muffle furnace at 500 ℃ for 4 hours to remove the sodium carboxymethyl cellulose, and then is subjected to air firing in a hot pressing furnace at 1950 ℃ for 4 hours to obtain the silicon carbide ceramic skeleton with the sheet-mounted oriented pore structure.
Through the shell of the embodiment, the highly ordered ceramic skeleton in the compound with the shell-like structure serves as a good heat conduction channel, so that the heat conduction coefficient is large, and heat can be rapidly stored. And the compound of the shell-like structure has the property of an interlayer structure, so that the mechanical strength of the compound is enhanced, the preparation method is simple, the cost is low, the adjustability is wide, the compound can be adjusted according to various application scenes, and the compound material is non-toxic and pollution-free
Based on the above, the invention utilizes the freeze drying technology to prepare the ceramic framework with the multilayer flaky hole, and then utilizes the capillary adsorption effect of the porous framework to fill the molten phase change material in the flaky hole interlayer, so as to form the composite phase change material with the shell-like interlayer structure, wherein the inorganic mineral layer on the surface of the shell corresponds to the ceramic framework and the organic protein layer corresponds to the phase change heat storage material, the ceramic framework has higher heat conductivity coefficient, and the bionic structure of the shell-like shell is obtained, so that the composite phase change material has the advantages of large heat storage density, high heat conductivity coefficient and high structural strength, and has better application prospects in the fields of solar energy utilization, building heating, industrial waste heat utilization and the like.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A shell-like structure bionic composite phase-change heat storage material is characterized by comprising a sheet-shaped pore structure ceramic framework, a ceramic additive and a phase-change material soaked in pores of the ceramic framework; the porosity of the sheet-shaped pore structure ceramic framework is 50-85%, the mass percent of the ceramic additive is 0-10%, and the volume percent of the ceramic framework in the composite phase-change heat storage material is 15-50%;
the phase-change material is one or more than two of organic phase-change material sugar alcohols and inorganic phase-change material inorganic salts; the ceramic framework is made of SiC, AlN, Al2O3, MgO, TiN or SiO2 as a base material; the ceramic additive is one or a plurality of combination modes of yttrium oxide, aluminum oxide, lanthanum oxide, sodium carboxymethylcellulose, polyvinyl alcohol and sodium dodecyl benzene sulfonate.
2. The shell-like structure and shell-like structure bionic composite phase-change heat storage material as claimed in claim 1, wherein the phase-change material is selected from 1 or more than 2 of lipid, sugar alcohol, nitrate, carbonate and chloride.
3. The shell-like structure bionic composite phase-change heat storage material of claim 2,
the sugar alcohol is erythritol, mannitol or paraffin; such as lithium nitrate, sodium chloride or lithium carbonate.
4. A method for preparing a bionic composite phase-change heat storage material with a shell-like structure according to any one of claims 1 to 3, which is characterized by comprising the following steps:
(1) uniformly mixing ceramic powder and a ceramic additive, adding deionized water, and ball-milling and uniformly mixing to form ceramic slurry;
(2) removing bubbles of the ceramic slurry obtained in the step (1) in vacuum, pouring the ceramic slurry into a customized mould, and pre-freezing and drying the ceramic slurry in a freeze dryer to obtain a ceramic blank;
(3) discharging the ceramic additives from the ceramic blank in the step (2) at low temperature, and sintering the ceramic blank in a high-temperature furnace in inert atmosphere without pressure;
(4) melting the phase-change material in a high-temperature atmosphere above the melting point and below the volatilization point;
(5) transferring the melt in the step (4) to a vacuum environment, putting the ceramic skeleton obtained in the step (3) into the vacuum environment, and carrying out vacuum infiltration for 0.5-3 h;
(6) and taking out the sample, and polishing and grinding the surface of the sample to obtain the bionic composite phase-change heat storage material with the shell-like structure.
5. The shell-like structure bionic composite phase-change heat storage material of claim 4, wherein the ceramic skeleton is one or a combination of at least two of SiC, AlN, Al2O3, MgO, TiN and SiO 2.
6. The method of claim 4, wherein the ceramic additive is one or more of yttria, alumina, lanthana, sodium carboxymethylcellulose, polyvinyl alcohol, sodium dodecylbenzenesulfonate.
7. The method according to claim 4, wherein the volume ratio of the ceramic powder to the deionized water is 1:9 to 2:3, i.e., the solid content is 10vol% to 40 vol%.
8. The preparation method of claim 1, wherein the ball milling rotation speed is 100r/min to 900r/min, and the ball milling time is 0.5h to 12 h.
9. The preparation method of claim 1, wherein the freeze drying prefreezing temperature is-90 ℃ to-20 ℃, the bottom of the mold is sealed by a metal bottom plate with high thermal conductivity coefficient, the metal bottom plate with high thermal conductivity coefficient is a copper sheet, the periphery of the side surface of the metal bottom plate is made of a material with low thermal conductivity coefficient, the material with low thermal conductivity coefficient is polytetrafluoroethylene or PMMA, and the top of the metal bottom plate is open.
10. The method of claim 4, wherein the sintering inert atmosphere is nitrogen or argon, and the sintering temperature is 1400 ℃ to 2050 ℃; the volume ratio of the phase-change material to the ceramic framework is 1: 2-5: 1, and the content of the single ceramic additive accounts for 0-5% of the mass of the ceramic powder.
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| CN114292628A (en) * | 2021-12-13 | 2022-04-08 | 南京航空航天大学 | Bamboo-like phase-change heat storage material and preparation method thereof |
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| CN116005056A (en) * | 2022-12-06 | 2023-04-25 | 宁波大学 | Ceramic-based metal microcapsule/organic phase change composite material and preparation method thereof |
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| CN116589299A (en) * | 2023-05-05 | 2023-08-15 | 哈尔滨工业大学 | Porous silicon carbide ceramic framework with bionic annual ring structure, preparation method thereof and application thereof in high-performance composite phase change material |
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Application publication date: 20210402 |