CN114717437A - Preparation method and application of aluminum-based metal high-temperature phase change heat storage composite material - Google Patents

Preparation method and application of aluminum-based metal high-temperature phase change heat storage composite material Download PDF

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CN114717437A
CN114717437A CN202111180274.XA CN202111180274A CN114717437A CN 114717437 A CN114717437 A CN 114717437A CN 202111180274 A CN202111180274 A CN 202111180274A CN 114717437 A CN114717437 A CN 114717437A
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aluminum
based metal
heat storage
temperature
change heat
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朱春宇
施松岑
盛楠
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China University of Mining and Technology CUMT
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    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
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    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02—Materials undergoing a change of physical state when used
    • C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/12—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/14—Thermal energy storage

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Abstract

The invention discloses a preparation method and application of an aluminum-based metal high-temperature phase-change heat storage composite material, which comprises the steps of firstly, boiling a mixture of micron-sized aluminum-based metal particles and aluminum oxide or aluminum hydroxide particles in boiling water to enable the surfaces of the aluminum-based metal particles to generate hydrolysis reaction to form an oxide precursor shell film, and fully mixing the oxide precursor shell film with the aluminum oxide or aluminum hydroxide particles; secondly, placing the dried mixture in a mould for compression molding; and finally, carrying out high-temperature heat treatment on the pressed sample in an oxygen-containing atmosphere to prepare the shaped composite phase change heat storage material of the aluminum-based metal and the aluminum oxide. The composite phase-change material prepared by the invention can effectively prevent the leakage of aluminum-based metal after melting, and has the advantages of high heat storage density, long cycle service life and the like.

Description

Preparation method and application of aluminum-based metal high-temperature phase change heat storage composite material
Technical Field
The invention relates to the field of heat storage and heat energy utilization, in particular to a preparation method and application of an aluminum-based metal high-temperature phase-change heat storage composite material.
Background
In recent years, under the drive of increasingly serious international environmental energy crisis and national energy conservation and emission reduction, the problems of mismatching of energy demand and supply in space and time, low energy utilization rate and the like can be effectively solved by applying the phase-change heat storage technology. The phase-change heat storage technology has wide application prospect in the fields of industrial waste heat recovery, building heat preservation and refrigeration, solar heat utilization and the like.
The phase change heat storage is to utilize phase change material to absorb or release heat in the phase change process, thereby achieving the purposes of heat storage and release, and utilizing the heat to adjust the energy demand and supply. Common solid-liquid phase change materials mainly comprise inorganic water, salt, organic phase change materials, molten salt, metal phase change materials and the like. Most phase-change energy storage materials have some problems, for example, the phase-change process of inorganic hydrous salt phase-change materials has the defects of high supercooling degree and phase separation, so that the materials are precipitated and separated, and the phase-change energy storage materials cannot be widely applied in industry; the molten salt phase change material has relatively more defects, such as large change rate of phase change volume, high supercooling degree, low thermal conductivity, high corrosivity and the like; organic phase change materials have low thermal conductivity, low phase change temperatures and are not extensive. In contrast, the metal phase-change material has the advantages of high energy storage density, high use temperature, suitability for high-temperature heat storage, good thermal stability, high thermal conductivity, no phase separation phenomenon, high cost performance and the like, so that the metal phase-change material can stand out from various phase-change materials, but has the problems of liquid phase leakage, high-temperature corrosion and the like, thereby limiting the wide application of the metal phase-change material in many fields. Therefore, if the metal phase change material can be packaged and shaped, the problems of leakage and corrosion can be effectively solved, and the method can be popularized and applied to the fields of solar thermal power generation, industrial waste heat recycling and the like.
Disclosure of Invention
The invention aims to provide a preparation method of an aluminum-based metal high-temperature phase-change heat storage composite material, which can solve the problems of liquid phase leakage, high-temperature corrosion and the like of a metal phase-change material after high-temperature melting and phase change.
The second purpose of the invention is to provide the application of the metal phase change heat storage composite material prepared by the method.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of an aluminum-based metal phase-change heat storage composite material comprises the following steps:
1) carrying out water boiling treatment on aluminum-based metal particles and aluminum oxide or aluminum hydroxide particles in a certain ratio in boiling water, carrying out hydrolysis reaction on the surfaces of the aluminum-based metal particles to form an oxide precursor shell film, and fully mixing the oxide precursor shell film with the aluminum oxide or aluminum hydroxide particles;
2) drying the mixture, and then putting the mixture into a mould for compression molding treatment to prepare a mixture blank with a certain shape;
3) and carrying out high-temperature heat treatment on the pressed blank sample in an oxygen-containing atmosphere to prepare the shaped composite phase change heat storage material of the aluminum-based metal and the aluminum oxide.
Preferably, the preparation method of the aluminum-based metal high-temperature phase change heat storage composite material is characterized in that the aluminum-based metal particles are selected from aluminum metal simple substance and one or more of binary or multi-element aluminum alloys such as aluminum-silicon alloy, aluminum-magnesium alloy, aluminum-copper alloy, aluminum-zinc alloy, aluminum-copper-silicon alloy, aluminum-magnesium-copper-tin alloy and the like.
Preferably, the preparation method of the aluminum-based metal high-temperature phase change heat storage composite material is characterized in that the particle size of the aluminum-based metal is 1-100 μm, and the size of the aluminum oxide or aluminum hydroxide is 5nm-100 μm.
Preferably, the preparation method of the aluminum-based metal high-temperature phase change heat storage composite material is characterized in that the mass percentage of the aluminum-based metal particles is 20-100%.
Preferably, the preparation method of the aluminum-based metal high-temperature phase change heat storage composite material is characterized in that the water boiling treatment time in the step (1) is 0.5-20 hours.
Preferably, the preparation method of the aluminum-based metal high-temperature phase change heat storage composite material is characterized in that the pressure of the sample in the step (2) during compression molding is 2-200 MPa.
Preferably, the preparation method of the aluminum-based metal high-temperature phase change heat storage composite material is characterized in that the shape of the sample pressed and formed in the step (2) is spherical, square, cylindrical and the like.
Preferably, the preparation method of the aluminum-based metal high-temperature phase change heat storage composite material is characterized in that the high-temperature heat treatment temperature in the step (3) is 700-1200 ℃, the treatment time is 0.5-20 hours, and the treatment atmosphere is air or oxygen.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention generates a layer of corresponding metal oxide precursor shell film on the surface of metal particles by a simple water boiling treatment method, fully mixes the metal oxide precursor shell film with a certain amount of aluminum oxide/aluminum hydroxide particles, carries out high-temperature heat treatment in an oxygen-containing atmosphere after compression molding, and carries out sintering and shaping on the oxide precursor shell film formed by water boiling and the aluminum oxide/aluminum hydroxide mixed particles during the high-temperature heat treatment to form a matrix network formed by oxides and wrap the metal particles in the matrix network, thereby effectively preventing the leakage of molten aluminum-based metal and finally forming the stable shaped composite phase-change material of the aluminum-based metal and the oxides. The metal particles are wrapped in the oxide matrix network to isolate the metal particles from the outside, so that the service life of the metal particles is longer.
2. The preparation method is simple and convenient, the process cost is low, and the obtained metal phase-change heat storage material has excellent heat storage performance.
3. The method has the advantages of easy acquisition by using water as a reagent, no generation of harmful substances in the reaction, zero environmental pollution and the like.
Drawings
FIGS. 1(a) and (b) are SEM morphology comparison graphs of Al-Si alloy particles with sizes of 30-45 μm before and after boiling treatment, respectively.
FIG. 2(a) is a schematic diagram of a composite sample after a boiling treatment and a high-temperature calcination treatment, and FIG. 2(b) is a schematic diagram of a composite sample after calcination treatment without a boiling treatment.
FIGS. 3(a) and (b) are DSC charts of the samples obtained in examples 1 and 2, respectively.
FIGS. 4(a) and (b) are a comparison of the physical images of the samples obtained in example 6 before and after 100 cycles, respectively.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Example 1
10g of 30-45 mu m aluminum-silicon alloy particles are placed in boiling water for boiling treatment for 2 hours, and then the moisture is evaporated, wherein figure 1 is a comparison of morphology graphs of the aluminum-silicon alloy particles before and after the boiling treatment, a precursor shell film of aluminum oxide is formed on the surfaces of the particles after the boiling treatment, and the surfaces of the particles are roughened. And (3) putting 0.5g of dried sample into a cylindrical die, pressing the dried sample into a cylindrical sample under the pressure of 5MPa by using a small powder tablet press, finally heating the cylindrical sample to 1000 ℃ at the heating rate of 2 ℃/min in an oxygen atmosphere, keeping the temperature for 2h, and cooling to room temperature at the cooling rate of 2 ℃/min to obtain the compound product. FIG. 2(a) is a pictorial representation of a sample that was prepared and which did not leak after high temperature heat treatment, illustrating the successful formation of a shaped composite phase change material. As a comparative experiment, when the al-si alloy pellets were directly press-molded without being subjected to the water-boiling treatment and subjected to the same heat treatment process, the sample exhibited al-si metal leakage, as shown in fig. 2 (b).
Example 2
10g of 30-45 mu m aluminum-silicon alloy particles are placed in boiling water for boiling treatment for 3 hours, after water is evaporated to dryness, 0.5g of dried sample is placed in a cylindrical die and pressed into a cylinder under the pressure of 10MPa by a small-sized powder tablet machine, finally, the cylindrical sample is heated to 1000 ℃ at the heating rate of 2 ℃/min in the oxygen atmosphere, the temperature is kept for 2 hours at constant temperature, and then the cylindrical sample is cooled to room temperature at the cooling rate of 2 ℃/min to prepare the compound product. FIG. 3 is a DSC test result of samples prepared in examples 1 and 2, wherein the melting temperature of the phase-change composite is 570.6 ℃ and 571.9 ℃, the phase-change solidification temperature is 559.0 ℃ and 560.1 ℃, the enthalpy of melting and heat absorption is 192.6J/g and 218.2J/g, and the enthalpy of heat release is 193.5J/g and 225.4J/g, so that the enthalpy of the obtained phase-change composite is higher and has a certain utilization value.
Example 3
10g of 30-micron aluminum-silicon alloy particles are placed in boiling water to be boiled for 2 hours, after water is evaporated to dryness, 1.5g of dried sample is placed in a spherical mold and pressed into a spherical shape under the pressure of 5MPa of an isostatic pressing machine, finally the spherical sample is heated to 1000 ℃ at the heating rate of 2 ℃/min in the oxygen atmosphere, the temperature is kept for 2 hours at constant temperature, and then the spherical sample is cooled to the room temperature at the cooling rate of 2 ℃/min, so that the complete and leak-free composite product is successfully prepared.
Example 4
10g of 100 mu m aluminum-silicon alloy particles are placed in boiling water for boiling for 20 hours, after the water is evaporated to dryness, 1.5g of dried sample is taken and placed in a spherical mold, the sample is pressed into a spherical shape under the pressure of 10MPa of a manual isostatic pressing machine, finally the spherical sample is heated to 1000 ℃ at the heating rate of 2 ℃/min in the oxygen atmosphere, the temperature is kept for 2 hours at constant temperature, and then the sample is cooled to the room temperature at the cooling rate of 2 ℃/min to obtain the compound product.
Example 5
5g of 1 mu m aluminum-silicon alloy particles and 5g of 50nm aluminum oxide particles are placed in boiling water for boiling for 0.5 hour, after the water is evaporated, 0.5g of dried sample is placed in a cylindrical die and pressed into a cylinder under the pressure of 2MPa of a small powder tablet press, finally, the cylindrical sample is heated to 700 ℃ at the heating rate of 2 ℃/min in the air atmosphere, the temperature is kept for 1 hour at constant temperature, and then the cylindrical sample is cooled to room temperature at the cooling rate of 2 ℃/min, thus obtaining the composite product.
Example 6
5g of 30-45 mu m aluminum-silicon alloy particles and 5g of 10nm aluminum oxide particles are put into boiling water for water boiling treatment for 2 hours, after water is evaporated, 0.5g of dried sample is put into a cylindrical die and pressed into a cylinder shape under the pressure of 10MPa of a small powder tablet machine, finally, the cylindrical sample is heated to 1000 ℃ at the heating rate of 2 ℃/min in the oxygen atmosphere, the temperature is kept for 2 hours at constant temperature, and then the cylindrical sample is cooled to room temperature at the cooling rate of 2 ℃/min to prepare the composite product. The sample is placed in an air atmosphere to carry out a melting and solidifying cycle experiment for 100 times, the cycle temperature is 520-620 ℃, the cycle temperature rise and fall rate is 2 ℃/min, and the sample is still intact after the cycle, as shown in fig. 4, the sample is compared with a real object image before and after the cycle of 100 times.
Example 7
9g of 5-micron aluminum metal particles and 1g of 100-micron aluminum hydroxide particles are placed in boiling water for boiling for 1 hour, after water is evaporated, 0.5g of dried sample is placed in a cylindrical die and pressed into a cylinder under the pressure of 5MPa of a small powder tablet press, finally, the cylindrical sample is heated to 900 ℃ at the heating rate of 1 ℃/min in the oxygen atmosphere, the temperature is kept for 1 hour at constant temperature, and then the cylindrical sample is cooled to room temperature at the cooling rate of 1 ℃/min, so that a compound product is prepared.
Example 8
2g of 100-micron aluminum-silicon alloy particles and 8g of 100-micron aluminum oxide particles are placed in boiling water for boiling for 10 hours, after water is evaporated, 0.5g of dried sample is placed in a cylindrical die and pressed into a cylinder under the pressure of 200MPa of a small powder tablet press, finally, the cylindrical sample is heated to 1200 ℃ at the heating rate of 0.5 ℃/min in the oxygen atmosphere, the temperature is kept for 20 hours at constant temperature, and then the cylindrical sample is cooled to the room temperature at the cooling rate of 2 ℃/min, so that a compound product is prepared.
Example 9
Placing 7.5g of 50-micron aluminum-silicon-copper alloy particles and 2.5g of 100-nm alumina particles in boiling water for boiling for 20 hours, drying the aluminum-silicon-copper alloy particles by evaporation, placing 0.5g of dried sample in a cylindrical die, pressing the sample into a cylinder under the pressure of 50MPa of a small powder tablet press, heating the cylindrical sample to 1000 ℃ at the heating rate of 1 ℃/min in an oxygen atmosphere, keeping the temperature for 10 hours, and cooling to room temperature at the cooling rate of 2 ℃/min to obtain the composite product.

Claims (9)

1. The preparation method of the aluminum-based metal high-temperature phase change heat storage composite material is characterized by comprising the following steps of:
1) carrying out water boiling treatment on aluminum-based metal particles and aluminum oxide or aluminum hydroxide particles in a certain ratio in boiling water, so that the surfaces of the aluminum-based metal particles are subjected to hydrolysis reaction to form an oxide precursor shell film, and the oxide precursor shell film is fully mixed with the aluminum oxide or aluminum hydroxide particles;
2) drying the mixture, and then putting the mixture into a mould for compression molding treatment to prepare a mixture blank with a certain shape;
3) and carrying out high-temperature heat treatment on the pressed blank sample in an oxygen-containing atmosphere to prepare the shaped composite phase change heat storage material of the aluminum-based metal and the aluminum oxide.
2. The method for preparing the aluminum-based metal high-temperature phase-change heat storage composite material as claimed in claim 1, wherein the aluminum-based metal particles are selected from aluminum metal simple substance, and one or more of binary or multi-element aluminum alloys such as aluminum-silicon alloy, aluminum-magnesium alloy, aluminum-copper alloy, aluminum-zinc alloy, aluminum-copper-silicon alloy, aluminum-magnesium-copper-tin alloy and the like.
3. The method for preparing the aluminum-based metal high-temperature phase-change heat storage composite material as claimed in claim 1, wherein the particle size of the aluminum-based metal is 1-100 μm, and the size of the aluminum oxide or aluminum hydroxide is 5nm-100 μm.
4. The method for preparing the aluminum-based metal high-temperature phase-change heat storage composite material as claimed in claim 1, wherein the mass ratio of the aluminum-based metal particles is 20-100%.
5. The method for preparing the aluminum-based metal high-temperature phase-change heat storage composite material as claimed in claim 1, wherein the water boiling treatment time in the step (1) is 0.5-20 hours.
6. The method for preparing the aluminum-based metal high-temperature phase change heat storage composite material as claimed in claim 1, wherein the pressure of the sample in the step (2) during compression molding is 2-200 MPa.
7. The method for preparing the aluminum-based metal high-temperature phase change heat storage composite material as claimed in claim 1, wherein the shape of the sample pressed in the step (2) is spherical, square, cylindrical, etc.
8. The method as claimed in claim 1, wherein the high temperature heat treatment temperature in step (3) is 700-1200 ℃, the treatment time is 0.5-20 hours, and the treatment atmosphere is air or oxygen.
9. The use of the aluminum-based metal high-temperature phase change heat storage composite material prepared by the preparation method of any one of claims 1 to 8 in a high-temperature heat storage system.
CN202111180274.XA 2021-10-11 2021-10-11 Preparation method and application of aluminum-based metal high-temperature phase change heat storage composite material Pending CN114717437A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101148577A (en) * 2007-10-18 2008-03-26 昆明理工大学 Aluminum/aluminum oxide base composite phase transition thermal storage material
CN109796937A (en) * 2019-01-04 2019-05-24 武汉科技大学 A kind of major diameter phase-transition heat-storage particle and preparation method thereof
CN111944491A (en) * 2020-08-21 2020-11-17 中国矿业大学 Preparation method and application of metal phase change microcapsule heat storage particles

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101148577A (en) * 2007-10-18 2008-03-26 昆明理工大学 Aluminum/aluminum oxide base composite phase transition thermal storage material
CN109796937A (en) * 2019-01-04 2019-05-24 武汉科技大学 A kind of major diameter phase-transition heat-storage particle and preparation method thereof
CN111944491A (en) * 2020-08-21 2020-11-17 中国矿业大学 Preparation method and application of metal phase change microcapsule heat storage particles

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