CN113275556B - Sn-based multi-element metal microsphere with low supercooling degree and preparation method thereof - Google Patents
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Abstract
The invention discloses an Sn-based multi-element metal microsphere with low supercooling degree and a preparation method thereof, wherein the Sn-based multi-element metal microsphere is an Sn-Zn-Cu ternary element metal microsphere, and the content of each metal element is as follows in mole percent: 82-96% of Sn, 1.5-2.5% of Cu and 2.5-15.5% of Cu. The preparation method of the Sn-Cu-Zn metal microsphere comprises the following steps: under the protection of inorganic molten salt, smelting three metals of Sn-Zn-Cu at high temperature to uniformly disperse Zn and Cu in Sn; ultrasonic emulsification is carried out to lead the metal to be dispersed in the inorganic fused salt to form metal emulsion; and rapidly cooling the emulsion, and washing to remove inorganic salt in the obtained solid to obtain the Sn-Cu-Zn metal microsphere. The particle size of the Sn-Cu-Zn metal microsphere prepared by the method is several micrometers to several tens micrometers, the melting point of the metal microsphere can be adjusted by changing the components of the microsphere, and the supercooling degree of the metal microsphere can be lower than 5 ℃. The Sn-Cu-Zn metal microsphere can be used as a solid-liquid phase change material for latent heat storage.
Description
Technical Field
The invention belongs to the technical field of phase change material preparation, and particularly relates to a Sn-based multi-element metal phase change material with low supercooling degree and a preparation method thereof.
Background
The energy is closely related to the production and life of human beings, and the improvement of the energy utilization efficiency is a key for ensuring the sustainable development of national economy and society. Among the methods for improving the energy utilization rate, energy storage technology is widely paid attention to and rapidly developed, wherein the most widely used technology is thermal energy storage, namely heat storage technology. The latent heat storage is realized by utilizing the phase change material to release/absorb heat when the physical state changes, the whole process is similar to constant temperature phase change, and the phase change material has the advantages of large energy storage capacity, high heat storage density, stable chemical property, low cost and the like, so that the phase change material has wide application in various fields. Solid-liquid phase change materials are a class of materials that can store or release thermal Energy during melting or crystallization, widely used in the field of latent heat storage, and include organic substances such as alkanes (y. Yuan, n. Zhang, et al Renewable and Sustainable Energy Reviews, 2014, 29, 482-498) and fatty acids (m.m. Kenisarin, solar Energy, 2014, 107, 553-575) and the like, as well as inorganic substances such as salts (q. Li, c.li, et al Applied Energy, 2019, 255, 13806-113842) and metals (a.i. Fern) and ndez, c.barrene che, et al Solar Energy Materials and Solar Cells, 2017, 171, 275-281) and the like. Compared with organic matters and inorganic salts, the metal serving as the phase change material has the advantages of large phase change enthalpy value (particularly high energy storage capacity per unit volume), high solid-liquid heat conductivity coefficient, relatively low vapor pressure, small thermal expansion, high thermal stability and the like.
Tin is a potential phase change material as a non-toxic, high density metal (s.zhu, m.t. Nguyen, et al ACS Applied Nano Materials, 2019, 2, 3752-3760). However, for pure Sn, especially small-sized micro-or nano-tin, an extremely high degree of supercooling is required for the liquid-solid phase change to occur, and the degree of supercooling is closely related to the size. For example, the supercooling degree of micrometer tin particles is related to the particle size, and when the size is reduced from 640 μm to 460 μm, the supercooling degree is increased from 50 ℃ to 95 ℃ (b.yang, y.l. Gao, et al, chinese Science Bulletin, 2010, 55, 2063-2065). If the supercooling degree exceeds the operating temperature range of the system, the latent heat thereof cannot be fully utilized, so that too high a supercooling degree of micro Sn hinders their practical application as phase change materials. Although another metal element (e.g., cu, co, or Ni) may be introduced into large-sized bulk Sn as impurities by a high-temperature calcination method, which may cause heterogeneous nucleation to reduce supercooling degree of bulk Sn (g. Parks, a. Faucet, et al Journal of Metals, 2014, 66, 2311-2319), such a high-temperature calcination method cannot produce Sn microspheres. In addition, since Sn supercooling is size dependent, the addition of only one metal element may not be sufficient to significantly reduce the supercooling of micro Sn. However, how to add various metal elements to reduce the supercooling degree of micro Sn and how to prepare such Sn-based multi-element metal microspheres are not yet disclosed in the literature (including patents).
Disclosure of Invention
Aiming at the technical problems existing in the prior art, the invention aims to provide Sn-based multielement metal microsphere with low supercooling degree and a preparation method thereof.
The Sn-based multi-element metal microsphere with low supercooling degree is characterized by being Sn-Zn-Cu ternary element metal microsphere.
The Sn-based multi-element metal microsphere with low supercooling degree is characterized in that the content of each metal element in the Sn-Zn-Cu three-element metal microsphere is as follows in mole percent: 82-96% of Sn, 1.5-2.5% of Cu and 2.5-15.5% of Cu.
The Sn-based multi-element metal microsphere with low supercooling degree is characterized in that the particle size of the Sn-Cu-Zn metal microsphere is from a few micrometers to tens of micrometers, and preferably 2-25 micrometers.
The preparation method of the Sn-Zn-Cu three-element metal microsphere with low supercooling degree is characterized by comprising the following steps of:
1) Smelting three metals of Sn, cu and Zn in molten salt: respectively placing the Sn particles, the Cu nanowires and the LiCl-KCl-CsCl eutectic mixture in a container protected by inert gas, heating to 700-800 ℃, stirring and maintaining for 10-30 min; then cooling to 550-650 ℃, adding Zn particles, stirring and maintaining for 40-80 min; stopping heating and cooling to obtain a mixture of solid metal and chloride;
2) Ultrasonic emulsification forms a metal emulsion: transferring the mixture of the solid metal and the chloride obtained in the step 1) into a ultrasonic emulsification container protected by inert gas, heating to 550-650 ℃ to enable the mixture of the solid metal and the chloride to be remelted, maintaining for 10-15min, then cooling to 350-400 ℃ to carry out ultrasonic emulsification, and dispersing the liquid metal into inorganic molten salt under the action of ultrasonic waves to form metal emulsion;
3) Removal of chloride: and 2) after the ultrasonic emulsification is finished, rapidly cooling the metal emulsion to room temperature, and washing to remove inorganic salt chloride in the obtained solid to obtain the Sn-Zn-Cu ternary element metal microsphere.
The method for preparing the Sn-Zn-Cu three-element metal microsphere with low supercooling degree is characterized by comprising the following specific process of step 1): respectively placing the Sn particles, the Cu nanowires and the LiCl-KCl-CsCl eutectic mixture in a container protected by inert gas, heating to 750 ℃, stirring and maintaining for 20min; then cooling to 600 ℃, adding Zn particles, stirring and maintaining for 60min; stopping heating and cooling to obtain a mixture of solid metal and chloride.
The method for preparing the Sn-Zn-Cu three-element metal microsphere with low supercooling degree is characterized in that the ultrasonic emulsification time in the step 2) is 5-6 min, the ultrasonic power is 900-1000W, and the emulsification temperature is 380 ℃.
The method for preparing the Sn-Zn-Cu three-element metal microsphere with low supercooling degree is characterized in that the LiCl-KCl-CsCl eutectic mixture used in the step 1) comprises, by weight, 53-55% of CsCl, 29-32% of LiCl and 14-16% of KCl, and preferably comprises 54.4% of CsCl, 30.3% of LiCl and 15.3% of KCl.
Compared with the prior art, the invention has the beneficial effects that:
the particle size of the Sn-Cu-Zn metal microsphere prepared by the method is several micrometers to several tens micrometers, the melting point of the metal microsphere can be adjusted by changing the components of the microsphere, and the supercooling degree of the metal microsphere can be lower than 5 ℃. The Sn-based alloy micro powder with low supercooling degree can be used as a solid-liquid phase change material for latent heat storage.
Drawings
FIG. 1a is a scanning electron micrograph of Sn-Zn-Cu metal microspheres prepared in example 1;
FIG. 1b is a Differential Scanning Calorimetric (DSC) chart of Sn-Zn-Cu metal microspheres (silica coated) prepared in example 1;
FIG. 2a is a scanning electron micrograph of Sn metal microspheres prepared in comparative example 1;
FIG. 2b is a Differential Scanning Calorimetric (DSC) chart of Sn metal microspheres (after silica coating) prepared in comparative example 1;
FIG. 3a is a scanning electron micrograph of Sn-Cu metal microspheres prepared in comparative example 2;
FIG. 3b is a Differential Scanning Calorimetric (DSC) chart of Sn-Cu metal microspheres (after silica coating) prepared in comparative example 2.
Detailed Description
The invention will be further illustrated with reference to specific examples, but the scope of the invention is not limited thereto.
Example 1
3.05 g of Sn pellets and 0.027 g of Cu nanowires (average diameter: about 120. 120 nm, the same applies hereinafter) were weighed separately, and they were charged into a calcination vessel under argon gas protection, and 22.1g of LiCl-KCl-CsCl eutectic mixture (its composition content: 54.4. 54.4 wt% CsCl, 30.3. 30.3 wt% LiCl, and 15.3. 15.3 wt% KCl, the same applies hereinafter) was charged into the calcination vessel, and the temperature was raised to 750 ℃. After stirring and maintaining for 20min, the temperature was reduced to 600℃and then 0.077 g Zn particles were added, stirring and maintaining at 600℃for 1 h. After calcination is completed, the liquid mixture is then rapidly cooled. Transferring the obtained solid mixture of salt and metal into a quartz test tube protected by argon after cooling, heating to 600 ℃ to completely melt the salt, and cooling to 380 ℃ to carry out ultrasonic emulsification (ultrasonic power is 960W, ultrasonic is 5 min).
After the end of the ultrasound, the metal emulsion was rapidly cooled to room temperature within 1min, the chloride salt in the resulting solid was removed by water washing, and the Sn-Zn-Cu microspheres were obtained after drying, as can be seen from the scanning electron image (fig. 1 a) of which the diameter was about 2-20 mm. To prevent the melted metal microspheres from polymerizing together in DSC testing to affect the test results, the Sn-Zn-Cu microspheres are subjected to SiO 2 After coating, DSC (coating method, see document Y.W. Tian and W. Luo, et al Ultrasonics Sonochemistry 2021, 73:105484, supra) was measured and the melting point (i.e. endothermic peak-peak temperature) was about 225.5℃and the supercooling degree (defined as the difference between the melting onset temperature and the solidification onset temperature) was about 4.6℃as shown in FIG. 1 b.
Comparative example 1
3.0 g of Sn particles are weighed and added into a quartz test tube protected by argon, 22.1g of LiCl-KCl-CsCl eutectic mixture is added, the temperature is raised to 600 ℃ to completely melt the salt, and the temperature is reduced to 380 ℃ to carry out ultrasonic emulsification (the ultrasonic power is 960W, and the ultrasonic treatment is carried out for 5 min). After the ultrasonic treatment, the metal emulsion is rapidly cooled to room temperature within 1min, the chloride in the obtained solid is removed by water washing, and Sn microspheres are obtained after drying, and the scanning electron image is shown as figure 2a and is obtained through SiO 2 As shown in FIG. 2b, the DSC of the coated Sn microsphere has a melting point of about 231.9 ℃ and a supercooling degree of about 83.7 ℃ which is far higher than that of the Sn-Zn-Cu microsphere in example 1.
Comparative example 2
3.05 g of Sn particles and 0.027 g of Cu self-made nanowires were weighed separately and added to a calcination vessel under argon protection. 22.1g of LiCl-KCl-CsCl eutectic was then added to the calcination vessel and the temperature was increased to 750 ℃. After stirring and maintaining for 20min, the temperature was reduced to 600 ℃, and 1 h was stirred and maintained. After calcination is completed, the liquid mixture is then rapidly cooled. Transferring the obtained solid mixture of salt and metal into a quartz test tube protected by argon after cooling, heating to 600 ℃ to completely melt the salt, and cooling to 380 ℃ to carry out ultrasonic emulsification (ultrasonic power is 960W, ultrasonic is 5 min). After the end of the sonication, the metal emulsion was rapidly cooled to room temperature within 1 min. Washing the obtained solid with water to remove chloride, and drying to obtain Sn-Cu microsphere with scanning electron image as shown in FIG. 3a, via SiO 2 As shown in FIG. 3b, the DSC of the coated Sn-Cu microsphere has a melting point of about 230.3 ℃ and a supercooling degree of about 65.6 ℃, which is far higher than that of the Sn-Zn-Cu microsphere in example 1.
Example 2
3.0 g of Sn particles and 0.035 g of Cu self-made nanowires were weighed separately and added to a calcination vessel under argon protection. About 22.1g of LiCl-KCl-CsCl eutectic was then added to the calcination vessel and the temperature was raised to 750 ℃. After stirring and maintaining for 20min, the temperature was reduced to 600℃and then 0.079g Zn particles were added, stirring and maintaining at 600℃for 1 h. After calcination is completed, the liquid mixture is then rapidly cooled. After cooling, the solid mixture of salt and metal obtained is transferred to argon protectionAfter the temperature is raised to 600 ℃ to completely melt the salt, the temperature is reduced to 380 ℃ to carry out ultrasonic emulsification (ultrasonic power is 960W, ultrasonic is 5 min). After the end of the sonication, the metal emulsion was rapidly cooled to room temperature within 1 min. Washing the obtained solid with water to remove chloride, drying to obtain Sn-Zn-Cu microsphere, and passing through SiO 2 After coating, the Sn-Zn-Cu microspheres have a melting point of about 225.6 ℃ and a supercooling degree of about 4.7 ℃.
Example 3
3.06 g of Sn particles and 0.028 g of Cu self-made nanowires were weighed separately and added to a calcination vessel under argon protection. 22.1g of LiCl-KCl-CsCl eutectic was then added to the calcination vessel and the temperature was increased to 750 ℃. After stirring and maintaining for 20min, the temperature was lowered to 600℃and then 0.096 g of Zn pellets were added, stirring and maintaining at 600℃for 1 h. After calcination is completed, the liquid mixture is then rapidly cooled. Transferring the obtained solid mixture of salt and metal into a quartz test tube protected by argon after cooling, heating to 600 ℃ to completely melt the salt, and cooling to 380 ℃ to carry out ultrasonic emulsification (ultrasonic power is 960W, ultrasonic is 5 min). After the end of the sonication, the metal emulsion was rapidly cooled to room temperature within 1 min. Washing the obtained solid with water to remove chloride, drying to obtain Sn-Zn-Cu microsphere, and passing through SiO 2 After coating, the Sn-Zn-Cu microspheres have a melting point of about 225.4 ℃ and a supercooling degree of about 2.8 ℃.
Example 4
3.08 g of Sn particles and 0.028 g of Cu self-made nanowires were weighed separately and added to a calcination vessel under argon protection. 22.1g of LiCl-KCl-CsCl eutectic was then added to the calcination vessel and the temperature was increased to 750 ℃. After stirring and maintaining for 20min, the temperature was lowered to 600℃and then 0.29 g of Zn particles were added, stirring and maintaining at 600℃for 1 h. After calcination is completed, the liquid mixture is then rapidly cooled. Transferring the obtained solid mixture of salt and metal into a quartz test tube protected by argon after cooling, heating to 600 ℃ to completely melt the salt, and cooling to 380 ℃ to carry out ultrasonic emulsification (ultrasonic power is 960W, ultrasonic is 5 min). After the end of the sonication, the metal emulsion was rapidly cooled to room temperature within 1 min. Washing the obtained solid with water to remove chloride, drying to obtain Sn-Zn-Cu microsphere, and passing through SiO 2 After coating, the Sn-Zn-Cu microspheres have a melting point of about 199.1 ℃ and a supercooling degree of about 1.0 ℃.
Example 5
3.05 g of Sn particles and 0.027 g of Cu self-made nanowires were weighed separately and added to a calcination vessel under argon protection. 22.1g of LiCl-KCl-CsCl eutectic was then added to the calcination vessel and the temperature was increased to 750 ℃. After stirring and maintaining for 20min, the temperature was lowered to 600℃and then 0.057 g of Zn pellets were added, stirring and maintaining at 600℃for 1 h. After calcination is completed, the liquid mixture is then rapidly cooled. Transferring the obtained solid mixture of salt and metal into a quartz test tube protected by argon after cooling, heating to 600 ℃ to completely melt the salt, and cooling to 380 ℃ to carry out ultrasonic emulsification (ultrasonic power is 960W, ultrasonic is 5 min). After the end of the sonication, the metal emulsion was rapidly cooled to room temperature within 1 min. Washing the obtained solid with water to remove chloride, and drying to obtain Sn-Zn-Cu microsphere via SiO 2 After coating, the Sn-Zn-Cu microspheres have a melting point of about 230.1 ℃ and a supercooling degree of about 2.5 ℃.
What has been described in this specification is merely an enumeration of possible forms of implementation for the inventive concept and may not be considered limiting of the scope of the present invention to the specific forms set forth in the examples.
Claims (5)
1. The preparation method of the Sn-based multi-element metal microsphere with low supercooling degree is characterized in that the Sn-based multi-element metal microsphere is a Sn-Zn-Cu three-element metal microsphere, and the content of each metal element in the Sn-Zn-Cu three-element metal microsphere is as follows in mole percent: 82-96% of Sn, 1.5-2.5% of Cu and 2.5-15.5% of Zn;
the particle size of the Sn-Zn-Cu metal microspheres is 2-25 microns; the preparation method of the Sn-Zn-Cu three-element metal microsphere with low supercooling degree comprises the following steps:
1) Smelting three metals of Sn, cu and Zn in molten salt: respectively placing the Sn particles, the Cu nanowires and the LiCl-KCl-CsCl eutectic mixture in a container protected by inert gas, heating to 700-800 ℃, stirring and maintaining for 10-30 min; then cooling to 550-650 ℃, adding Zn particles, stirring and maintaining for 40-80 min; stopping heating and cooling to obtain a mixture of solid metal and chloride;
2) Ultrasonic emulsification forms a metal emulsion: transferring the mixture of the solid metal and the chloride obtained in the step 1) into a ultrasonic emulsification container protected by inert gas, heating to 550-650 ℃ to enable the mixture of the solid metal and the chloride to be remelted, maintaining for 10-15min, then cooling to 350-400 ℃ to carry out ultrasonic emulsification, and dispersing the liquid metal into inorganic molten salt under the action of ultrasonic waves to form metal emulsion;
the time of ultrasonic emulsification in the step 2) is 5-6 min, and the ultrasonic power is 900-1000W;
3) Removal of chloride: and 2) after the ultrasonic emulsification is finished, rapidly cooling the metal emulsion to room temperature within 0.8-1.5min, and washing to remove inorganic salt chloride in the obtained solid to obtain the Sn-Zn-Cu three-element metal microsphere.
2. The method for preparing the Sn-based multi-element metal microsphere with low supercooling degree according to claim 1, wherein the specific process of the step 1) is as follows: respectively placing the Sn particles, the Cu nanowires and the LiCl-KCl-CsCl eutectic mixture in a container protected by inert gas, heating to 750 ℃, stirring and maintaining for 20min; then cooling to 600 ℃, adding Zn particles, stirring and maintaining for 60min; stopping heating and cooling to obtain a mixture of solid metal and chloride.
3. The method for preparing a Sn-based multi-element metal microsphere with low supercooling degree according to claim 1, wherein the ultrasonic emulsification temperature in step 2) is 380 ℃.
4. The method for preparing the Sn-based multi-element metal microsphere with low supercooling degree according to claim 1, wherein the LiCl-KCl-CsCl eutectic mixture used in the step 1) comprises, by weight, csCl 53-55%, liCl 29-32% and KCl 14-16%.
5. The method of preparing Sn-based multi-element metal microspheres with low supercooling degree according to claim 4, wherein the content of LiCl-KCl-CsCl eutectic mixture is CsCl 54.4%, liCl 30.3% and KCl 15.3% by weight.
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