CN111548167A - Ceramic-based high-thermal-conductivity composite phase-change heat storage material and preparation method thereof - Google Patents
Ceramic-based high-thermal-conductivity composite phase-change heat storage material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ceramic-based high-thermal-conductivity composite phase-change heat storage material and a preparation method thereof, wherein the ceramic-based high-thermal-conductivity composite phase-change heat storage material comprises the following raw materials in percentage by mass: 50-70% of inorganic salt, 20-50% of aluminum nitride and 5-15% of water. Firstly, weighing inorganic salt and aluminum nitride according to a formula proportion, uniformly stirring, adding water, mixing and forming to prepare a composite phase-change heat storage material precursor; then placing the precursor sealing package device in a blast drying oven for low-temperature reaction to prepare a green body; and finally, heating and sintering the green body to obtain the ceramic-based high-thermal-conductivity composite phase-change heat storage material. According to the invention, the heat-conducting ceramic matrix framework is prepared in one step by an in-situ reaction method, the heat conductivity of the composite phase change material is greatly enhanced while the eutectic phase change salt is packaged, and the heat conductivity can reach more than 4W/m.K; the micron-sized raw materials are adopted, so that the production cost can be obviously reduced, and the method has the potential of industrial production.
Description
Technical Field
The invention relates to a ceramic-based high-thermal-conductivity composite phase-change heat storage material and a preparation method thereof, belonging to the technical field of phase-change material preparation.
Background
With the increasing shortage of energy supply and the increasing environmental protection pressure, phase-change materials are highly valued by people due to their unique characteristics and are applied to more and more fields, such as residential heating, steam production, waste heat recovery, and the like. The basic principle of the phase-change energy storage technology is to store energy through the isothermal phase-change process of materials and release the energy for use when needed, and the phase-change energy storage technology is an important means for solving the problem of mismatching of energy space and time.
In a phase-change material system, inorganic salts have a relatively proper melting point and relatively large phase-change latent heat, and attract extensive attention of various fields. However, the inorganic salt phase change material needs to solve two problems in the using process, namely material encapsulation is adopted, so that the corrosion to metal parts is reduced, and meanwhile, the modularized installation is convenient; secondly, strengthen heat conduction, improve the heat charge and discharge power, prevent local overtemperature. The common technical means at present is to compound the nanoscale adsorption material and graphite, but the production requirements are not satisfied enough, on one hand, the nanoscale adsorption material is expensive, and on the other hand, the graphite packaging process is high, so that potential safety hazards easily exist.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a ceramic-based high-thermal-conductivity composite phase-change heat storage material and a preparation method thereof.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the invention provides a ceramic-based high-thermal-conductivity composite phase-change heat storage material, which comprises the following components in percentage by mass:
50 to 70 percent of inorganic salt,
20 to 50 percent of aluminum nitride,
and the number of the first and second groups,
5 to 15 percent of water.
Further, the inorganic salt is Na2CO3、Li2CO3、CaCO3One or more of NaCl and KCl.
Furthermore, the aluminum nitride is industrial grade, and the granularity is 1-100 mu m.
The invention provides a preparation method of a ceramic-based high-thermal-conductivity composite phase-change heat storage material, which comprises the following steps:
(1) weighing inorganic salt and aluminum nitride according to the proportion of the raw materials, uniformly stirring, adding water, mixing and forming to prepare a composite phase-change heat storage material precursor;
(2) sealing and packaging the prepared precursor, and placing the precursor in a forced air drying oven for low-temperature reaction to prepare a green body;
(3) and placing the prepared green body in a muffle furnace, and heating and sintering to obtain the ceramic-based high-thermal-conductivity composite phase-change heat storage material.
Further, the raw materials comprise the following components in percentage by mass: 50-70% of inorganic salt, 20-50% of aluminum nitride and 5-15% of water.
Further, the inorganic salt is Na2CO3、Li2CO3、CaCO3One or more of NaCl and KCl.
Further, the molding pressure is 20-40MPa, and the pressure maintaining time is 1-5 min.
Further, the temperature of the air-blast drying oven is set to be 40-80 ℃, and the reaction time is 12-24 hours.
Further, the heating sintering process comprises the following steps: heating to 105 ℃ at a certain heating rate, and keeping the temperature for 0.5-2 h; heating to 280-350 ℃ at a certain heating rate, and preserving heat for 1-3 h; finally, heating to 500-800 ℃ at a certain heating rate, and preserving heat for 2-4 h; cooling to room temperature along with the furnace.
Further, the heating rate is 5-20 ℃/min.
The invention has the beneficial effects that:
(1) according to the preparation method of the ceramic-based high-heat-conductivity composite phase-change heat storage material, the high-heat-conductivity composite phase-change heat storage material is prepared in one step by means of physical mixing and in-situ reaction, so that the heat conduction material and the adsorption material are more uniformly distributed, the phase-change material is prevented from cracking due to thermal stress generated by uneven temperature, and the practical phase-change heat storage material with high heat conductivity and good cycle stability is obtained. The phase-change temperature of the developed phase-change material is 400-800 ℃, and the phase-change material is suitable for the fields of steam production, photo-thermal storage, waste heat recovery and the like.
(2) The invention adopts aluminum nitride as a heat-conducting base material, has stable performance, low expansion rate, oxidation resistance and corrosion resistance, solves the problem of high-temperature oxidation of the graphite-based material, and has the heat conductivity of more than 4W/m.K.
(3) The invention does not need nano material as adsorbent, thus greatly reducing the cost of raw materials; the preparation process is simple, the material source is wide, the preparation method is suitable for large-scale industrial production, and the preparation method has wide application prospects in multiple fields.
Drawings
FIG. 1 is a diagram of a sample of example 1 of the present invention with no water added; FIG. 1(a) is a schematic representation of a finished product prepared in example 1 without the addition of water; FIG. 1(b) is a pictorial representation of a finished product prepared in example 1 with water;
FIG. 2 is an SEM photograph of a phase change material prepared according to example 1 of the present invention;
FIG. 3 is a DSC curve of the phase change material prepared in example 1 of the present invention and pure phase change salt.
Detailed Description
The invention is further described below. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The invention provides a ceramic-based high-thermal-conductivity composite phase-change heat storage material, which comprises the following components in percentage by mass:
50 to 70 percent of inorganic salt,
20 to 50 percent of aluminum nitride,
and the number of the first and second groups,
5 to 15 percent of water.
Further, the inorganic salt is Na2CO3、Li2CO3、CaCO3One or more of NaCl and KCl.
Furthermore, the aluminum nitride is industrial grade, and the granularity is 1-100 mu m.
The invention also provides a preparation method of the ceramic-based high-thermal-conductivity composite phase-change heat storage material, which comprises the following steps:
(1) weighing inorganic salt and aluminum nitride according to a formula proportion, uniformly stirring, adding water, mixing and forming to prepare a composite phase-change heat storage material precursor;
(2) sealing and packaging the precursor prepared in the step (1), and placing the precursor in a forced air drying oven for low-temperature reaction to prepare a green body;
(3) and (3) placing the green body prepared in the step (2) in a muffle furnace, carrying out temperature programming, and heating and sintering to obtain the ceramic-based high-thermal-conductivity composite phase-change heat storage material.
Further, the formula comprises the following raw materials in percentage by mass: 50-70% of inorganic salt, 20-50% of aluminum nitride and 5-15% of water.
Further, the inorganic salt is Na2CO3、Li2CO3、CaCO3One or more of NaCl and KCl.
Furthermore, the aluminum nitride is industrial grade, and the granularity is 1-100 mu m.
Further, the molding pressure is 20-40MPa, and the pressure maintaining time is 1-5 min.
Further, the temperature of the air-blast drying oven is set to be 40-80 ℃, and the reaction time is 12-24 hours.
Further, the heating sintering process comprises the following steps: heating to 105 ℃ at a certain heating rate, and keeping the temperature for 0.5-2 h; heating to 280-350 ℃ at a certain heating rate, and preserving heat for 1-3 h; finally, heating to 500-800 ℃ at a certain heating rate, and preserving heat for 2-4 h; cooling to room temperature along with the furnace.
Further, the heating rate is 5-20 ℃/min.
Example 1
A ceramic-based high-thermal-conductivity composite phase-change heat storage material is prepared by the following steps: 2.6g of Li were weighed2CO3、3.4gNa2CO3And 4g of AlN powder is put into a powder grinding machine to be uniformly stirred, and then 1g of water is weighed and added into the powder grinding machine to be uniformly stirred. And pressing and molding the obtained mixed powder by using a press, wherein the pressure is 30MPa, and the pressure maintaining time is 3min, so as to obtain the precursor. And sealing and packaging the precursor, placing the precursor in a blast oven, and reacting at a low temperature for 16h, wherein the set temperature is 70 ℃. Transferring the obtained green body into a ceramic boat, placing the ceramic boat in a muffle furnace, heating to 105 ℃ at the heating rate of 5 ℃/min, and preserving heat for 1 h; then heating to 300 ℃ at the heating rate of 10 ℃/min, and preserving heat for 1.5 h; finally, heating to 550 ℃ at the heating rate of 5 ℃/min, and preserving heat for 2 h; cooling to room temperature along with the furnace.
Fig. 1(a) is a diagram of a finished product prepared without adding water, and fig. 1(b) is a diagram of a finished product prepared after adding water, and it can be seen that the finished product prepared without adding water cannot be formed.
Fig. 2 is an SEM image of the prepared phase change material, and it can be seen that the material has a dense structure.
Fig. 3 is a DSC curve of the prepared phase-change material with pure phase-change salt, and it can be seen that the material has a higher enthalpy of phase change.
Example 2
A ceramic-based high-thermal-conductivity composite phase-change heat storage material is prepared by the following steps: 2.6g of Li were weighed2CO3、3.4gNa2CO3And 3g of AlN powder is put into a powder grinding machine to be uniformly stirred, and then 1g of water is weighed and added into the powder grinding machine to be uniformly stirred. And pressing and molding the obtained mixed powder by using a press, wherein the pressure is 30MPa, and the pressure maintaining time is 3min, so as to obtain the precursor. And sealing and packaging the precursor, placing the precursor in a blast oven, and reacting at a low temperature for 16h, wherein the set temperature is 60 ℃. Transferring the obtained green body into a ceramic boat, placing the ceramic boat in a muffle furnace, heating to 105 ℃ at the heating rate of 5 ℃/min, and preserving heat for 1 h; then heating to 300 ℃ at the heating rate of 10 ℃/min, and preserving heat for 1.5 h; finally, heating to 550 ℃ at the heating rate of 5 ℃/min, and preserving heat for 2 h; followed byThe furnace is cooled to room temperature.
Example 3
A ceramic-based high-thermal-conductivity composite phase-change heat storage material is prepared by the following steps: weighing 2.6g of NaCl, 3.4g of KCl and 4g of AlN powder, putting the powder into a powdering machine, uniformly stirring, weighing 1g of water, adding the water into the powdering machine, and uniformly stirring. And pressing and molding the obtained mixed powder by using a press, wherein the pressure is 35MPa, and the pressure maintaining time is 3min, so as to obtain the precursor. And sealing and packaging the precursor, placing the precursor in a blast oven, and reacting at a low temperature for 16h, wherein the set temperature is 70 ℃. Transferring the obtained green body into a ceramic boat, placing the ceramic boat in a muffle furnace, heating to 105 ℃ at the heating rate of 5 ℃/min, and preserving heat for 1 h; then heating to 300 ℃ at the heating rate of 10 ℃/min, and preserving heat for 1.5 h; finally, heating to 750 ℃ at the heating rate of 5 ℃/min, and preserving heat for 2 h; cooling to room temperature along with the furnace.
Example 4
A ceramic-based high-thermal-conductivity composite phase-change heat storage material is prepared by the following steps: 2.6g of Li were weighed2CO3、3.4gNa2CO3And 4g of AlN powder is put into a powder grinding machine to be uniformly stirred, and then 1g of water is weighed and added into the powder grinding machine to be uniformly stirred. And pressing and molding the obtained mixed powder by using a press, wherein the pressure is 30MPa, and the pressure maintaining time is 1min, so as to obtain the precursor. And (3) sealing and packaging the precursor, placing the precursor in a blast oven for low-temperature reaction, wherein the set temperature is 40 ℃, and the reaction time is 24 h. Transferring the obtained green body into a ceramic boat, placing the ceramic boat in a muffle furnace, heating to 105 ℃ at the heating rate of 5 ℃/min, and preserving heat for 1 h; then heating to 300 ℃ at the heating rate of 10 ℃/min, and preserving heat for 1.5 h; finally, heating to 550 ℃ at the heating rate of 5 ℃/min, and preserving heat for 2 h; cooling to room temperature along with the furnace.
Example 5
A ceramic-based high-thermal-conductivity composite phase-change heat storage material is prepared by the following steps: 2.6g of Li were weighed2CO3、3.4gNa2CO3And 4g of AlN powder is put into a powder grinding machine to be uniformly stirred, and then 1g of water is weighed and added into the powder grinding machine to be uniformly stirred. And pressing and molding the obtained mixed powder by using a press, wherein the pressure is 30MPa, and the pressure maintaining time is 5min, so as to obtain the precursor. Sealing and packaging the precursor, placing the precursor in a blast oven for low-temperature reaction, and arrangingThe fixed temperature is 80 ℃, and the reaction time is 12 h. Transferring the obtained green body into a ceramic boat, placing the ceramic boat in a muffle furnace, heating to 105 ℃ at a heating rate of 10 ℃/min, and preserving heat for 1 h; then heating to 300 ℃ at the heating rate of 20 ℃/min, and preserving heat for 1.5 h; finally, heating to 550 ℃ at the heating rate of 10 ℃/min, and preserving heat for 2 h; cooling to room temperature along with the furnace.
Example 6
A ceramic-based high-thermal-conductivity composite phase-change heat storage material is prepared by the following steps: 2.6g of Li were weighed2CO3、3.4gNa2CO3And 4g of AlN powder is put into a powder grinding machine to be uniformly stirred, and then 1.5g of water is weighed and added into the powder grinding machine to be uniformly stirred. And pressing and molding the obtained mixed powder by using a press, wherein the pressure is 25MPa, and the pressure maintaining time is 3min, so as to obtain the precursor. And sealing and packaging the precursor, placing the precursor in a blast oven, and reacting at a low temperature for 20h at a set temperature of 50 ℃. Transferring the obtained green body into a ceramic boat, placing the ceramic boat in a muffle furnace, heating to 105 ℃ at the heating rate of 5 ℃/min, and preserving heat for 1 h; then heating to 300 ℃ at the heating rate of 10 ℃/min, and preserving heat for 1.5 h; finally, heating to 550 ℃ at the heating rate of 5 ℃/min, and preserving heat for 2 h; cooling to room temperature along with the furnace.
Comparative example 1
Referring to Chinese patent application No. 201610100879.6, a preparation method of a shaped medium-high temperature composite heat storage material comprises the following steps:
(1) processing vermiculite at 1300 ℃ for 20min, cooling, and mixing with a phase change material according to a mass ratio of 1:10, wherein the phase change material is MgCl with a weight ratio of 40.0-60.0%220.4-30.4 wt% of KCl and 19.6-29.6 wt% of NaCl, wherein the sum of the phase change materials is 100%;
(2) preserving the heat of the mixture for 6 hours at 400 ℃ and under the condition that the negative pressure is-15 kPa to prepare a composite phase-change material, mechanically crushing the composite phase-change material to 40 meshes, adding modified carbon fibers, and mechanically mixing for 24 hours, wherein the modified carbon fibers account for 2-8% of the total mass of the composite phase-change material;
(3) and (3) dropwise adding a high-temperature binder, pressing and forming under the pressure of 10-20 MPa, and finally, preserving heat at the temperature of 300 ℃ for 30min and curing to obtain the formed composite heat storage material for high temperature.
Comparative example 2
Referring to Chinese patent application No. 201711322736.0, a high-temperature phase-change composite heat storage ceramic-based material and a preparation method thereof, the preparation method comprises the following steps:
(1) mixing 20-30 parts of lithium carbonate, 20-30 parts of potassium carbonate, 30-40 parts of sodium carbonate and 10-15 parts of ceramic matrix, grinding to 400-500 meshes, and uniformly mixing to obtain an inorganic salt ceramic matrix system;
(2) heating 1-2 parts of high-thermal-conductivity carbon fiber and 1-2 parts of doped graphite in 500-600 ℃ inert gas for 15min, then adding the heated carbon fiber and the doped graphite into the inorganic salt ceramic matrix system, and grinding the mixture to 400-500 meshes for uniformly mixing to form a composite system;
(3) after the composite system is subjected to pressure forming, the pressure is 2.4-2.8 MPa, the pressure time is 2-2.5 min, the composite system is sintered for 20-30 min at 700-760 ℃, and the temperature is reduced to normal temperature after sintering is finished, so that the high-temperature phase-change composite heat storage ceramic-based material is obtained.
Comparative example 3
Referring to Chinese patent application No. 201710509716.8, a rare earth ceramic high-temperature phase change energy storage and release material and a preparation method thereof, the preparation method comprises the following steps:
(1) putting 92-98 parts of alumina, 5-8 parts of zirconia and rare earth oxide (with the aperture of 450-1000 nm-plus) solid solution, 1-3 parts of magnesia, 60-80 parts of cellulose solution and 100-plus 150 deionized water into a grinding machine for mixing and grinding to prepare mixed slurry, then injecting the mixed slurry into a mold for molding, and sintering at high temperature after the molded product is dried to prepare rare earth ceramic;
(2) mixing inorganic salt mixtures in the phase change materials, heating and melting at constant temperature to prepare mixed solution, then placing the rare earth ceramic in the mixed solution, boiling for 5-10 minutes, taking out the rare earth ceramic, placing the rare earth ceramic in a furnace with the temperature of 740-860 ℃ and naturally cooling along with the furnace to prepare the high-temperature phase change energy storage and release material of the rare earth ceramic.
The performance indexes of the phase-change heat storage material prepared by the embodiment of the invention are compared with the performance indexes of the phase-change material prepared by the comparative example as follows:
firstly, the thermal conductivity is tested as follows:
testing an instrument: hot Disk (TPS 2500) as tested according to ISO22007-2 standard, with the results as given in Table 1:
TABLE 1 partial examples and comparative examples thermal conductivity
As can be seen from Table 1, the heat conductivity coefficient of the high-heat-conductivity composite hydrated salt phase-change heat storage material prepared by the invention can reach more than 4W/m.K, is greatly higher than that of a comparative example, and has an engineering prospect.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The ceramic-based high-thermal-conductivity composite phase-change heat storage material is characterized by comprising the following components in percentage by mass:
50 to 70 percent of inorganic salt,
20 to 50 percent of aluminum nitride,
and the number of the first and second groups,
5 to 15 percent of water.
2. The ceramic-based high thermal conductivity composite phase change heat storage material of claim 1, wherein the inorganic salt is Na2CO3、Li2CO3、CaCO3One or more of NaCl and KCl.
3. The ceramic-based high thermal conductivity composite phase change heat storage material of claim 1, wherein the aluminum nitride is technical grade with a particle size of 1-100 μm.
4. A preparation method of a ceramic-based high-thermal-conductivity composite phase-change heat storage material is characterized by comprising the following steps:
(1) weighing inorganic salt and aluminum nitride according to the proportion of the raw materials, uniformly stirring, adding water, mixing and forming to prepare a composite phase-change heat storage material precursor;
(2) sealing and packaging the prepared precursor, and placing the precursor in a forced air drying oven for low-temperature reaction to prepare a green body;
(3) and placing the prepared green body in a muffle furnace, and heating and sintering to obtain the ceramic-based high-thermal-conductivity composite phase-change heat storage material.
5. The preparation method of the ceramic-based high-thermal-conductivity composite phase-change heat storage material according to claim 4, wherein the raw materials comprise, by mass: 50-70% of inorganic salt, 20-50% of aluminum nitride and 5-15% of water.
6. The method for preparing the ceramic-based high-thermal-conductivity composite phase-change heat storage material according to claim 4, wherein the inorganic salt is Na2CO3、Li2CO3、CaCO3One or more of NaCl and KCl.
7. The preparation method of the ceramic-based high-thermal-conductivity composite phase-change heat storage material according to claim 4, wherein the forming pressure is 20-40MPa, and the dwell time is 1-5 min.
8. The preparation method material of the ceramic-based high-thermal-conductivity composite phase-change heat storage material according to claim 4, wherein the set temperature of the air-blowing drying oven is 40-80 ℃, and the reaction time is 12-24 hours.
9. The preparation method of the ceramic-based high-thermal-conductivity composite phase-change heat storage material according to claim 4, wherein the heating and sintering process is as follows: heating to 105 ℃ at a certain heating rate, and keeping the temperature for 0.5-2 h; heating to 280-350 ℃ at a certain heating rate, and preserving heat for 1-3 h; finally, heating to 500-800 ℃ at a certain heating rate, and preserving heat for 2-4 h; cooling to room temperature along with the furnace.
10. The preparation method of the ceramic-based high-thermal-conductivity composite phase-change heat storage material according to claim 9, wherein the temperature rise rate is 5-20 ℃/min.
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