CN115319060B - Preparation method of high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material - Google Patents
Preparation method of high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
- B22D23/04—Casting by dipping
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/001—General methods for coating; Devices therefor
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/08—Alloys with open or closed pores
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
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Abstract
A preparation method of a high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material relates to a preparation method of a porous aluminum-based composite material. The problems that the existing glass bead aluminum-based porous composite material is low in strength and the existing glass beads cannot meet requirements are solved. The method comprises the following steps: weighing glass beads and the balance of aluminum ingots; weighing appropriate amount of alcohol, deionized water, ammonia water, formaldehyde and resorcinol, and mixing to obtain a solution; putting the glass beads into the solution, stirring, taking out the glass beads floating in the liquid, drying and sintering under a protective atmosphere to obtain the C-coated glass beads with the double-wall core-shell structure, then putting the C-coated glass beads into a mold for preheating, and putting the mold on the table top of a press for pressure infiltration. The strength of the glass microsphere Al porous composite material with the core-shell structure, which is prepared by coating the surfaces of the glass microspheres by a chemical method, is obviously improved.
Description
Technical Field
The invention relates to a preparation method of a porous aluminum matrix composite.
Background
The porous material is widely applied to the application field which needs high energy absorption because of light weight, high specific strength and large compression deformation, and the traditional porous material only mainly uses foam metal which cannot meet the requirement of energy absorption because of the problems of low strength, low rigidity and low impact load resistance. Therefore, a material engineer gains inspiration from a metal matrix composite material, introduces a material with hollow spheres into a metal matrix as a gap in a porous material, and the strength of the porous composite material prepared by the method is obviously improved compared with that of the traditional porous metal because the hollow material has certain strength, and the pore diameter of the gap introduced by the hollow material is controllable, so that the porous composite material has obvious advantages for material design, but because the strength of the existing hollow material such as glass beads is limited, the strength of the existing hollow material is generally increased by increasing the wall thickness and reducing the particle size, so that three problems exist: 1. increasing the wall thickness and reducing the particle size can significantly increase the density of the glass microspheres, leading to the density increase of the composite material and the increase of the specific strength thereof; 2. increasing the wall thickness and reducing the particle size can cause the porosity of the glass beads to be reduced, so that the porosity in the composite material can be reduced, and the energy absorption effect of the composite material can be influenced; 3. increasing the wall thickness and reducing the particle size can significantly increase the difficulty of composite material preparation.
Disclosure of Invention
The invention provides a preparation method of a high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material, aiming at solving the problems that the existing glass bead aluminum-based porous composite material is low in strength and the existing glass beads cannot meet the requirements.
The preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material comprises the following steps:
1. weighing;
weighing glass beads and the balance of aluminum ingots according to the volume fraction of 40-60%; weighing appropriate amount of alcohol, deionized water, ammonia water, formaldehyde and resorcinol, and mixing to obtain a solution;
the volume ratio of the alcohol to the deionized water to the ammonia water to the formaldehyde is 350 (15-45) to (2.8-5.6);
the mass ratio of the resorcinol to the formaldehyde is 1g: (1-2) mL;
2. preparing glass beads with a C-coated double-wall core-shell structure;
placing glass beads in the solution prepared in the first step, stirring for 12 hours by using a magnetic stirrer, taking out the glass beads floating in the liquid, drying in a vacuum drying oven, and sintering the dried powder in a tube furnace under a protective atmosphere to obtain C-coated glass beads with a double-wall core-shell structure;
the volume ratio of the mass of the glass beads to the volume of the solution prepared in the first step is 1g (10-50) mL;
the sintering temperature of the tubular furnace is 550-650 ℃;
the sintering time is 3-7 h;
3. preheating and preparing a metal matrix:
placing the glass beads with the double-wall core-shell structure coated by C obtained in the step two into a mold, directly compacting by using the gravity of the powder, and then moving the powder into a heating furnace for preheating to obtain a preheated prefabricated body; heating the aluminum ingot weighed in the step one to 250-450 ℃ above the melting point under the protective atmosphere to obtain a molten metal matrix;
4. liquid metal infiltration:
and (4) placing the preheated preform with the mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the preform in the mold, and performing pressure infiltration.
The invention has the beneficial effects that:
1. the invention adopts a chemical method to coat the surfaces of the glass beads, and can form polymer-shaped gel when a high-concentration alkaline catalyst is used, namely the obtained gel is formed by tightly connecting small particles, the connection area among the particles is larger, meanwhile, the gel has high specific surface area and high mechanical strength, the floating part in the solution is taken after the treatment process to ensure that the glass beads are complete, and meanwhile, the chemical treatment process can realize uniform and continuous coating on the surfaces of the glass beads.
2. The invention can regulate the thickness of the coated C shell by changing the PH value of the solution and the content of the reactant, and design the C shells with different coating thicknesses according to requirements.
3. The strength of the glass bead Al porous composite material with the core-shell structure prepared by the invention is obviously improved, wherein the peak stress is up to 190.2MPa, and the energy absorption capacity is up to 83.2MJ/cm 3 。
4. The invention adopts gravity compaction, does not need pressurization to prepare the prefabricated body, ensures the integrity of the glass beads as much as possible in the preparation process of the prefabricated body and ensures the integrity of the glass beads as much as possible.
Drawings
FIG. 1 is an SEM photograph of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material obtained in example 1.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, and any reasonable combination of the specific embodiments is included.
The first embodiment is as follows: the preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material comprises the following steps:
1. weighing;
weighing glass beads and the balance of aluminum ingots according to the volume fraction of 40-60%; weighing appropriate amount of alcohol, deionized water, ammonia water, formaldehyde and resorcinol, and mixing to obtain a solution;
the volume ratio of the alcohol to the deionized water to the ammonia water to the formaldehyde is 350 (15-45) to (2.8-5.6);
the mass ratio of the resorcinol to the formaldehyde is 1g: (1-2) mL;
2. preparing glass beads with a C-coated double-wall core-shell structure;
placing glass beads in the solution prepared in the first step, stirring for 12 hours by using a magnetic stirrer, taking out the glass beads floating in the liquid, drying in a vacuum drying oven, and sintering the dried powder in a tubular furnace under a protective atmosphere to obtain C-coated glass beads with a double-wall core-shell structure;
the volume ratio of the mass of the glass microspheres to the volume of the solution prepared in the first step is 1g (10-50) mL;
the sintering temperature of the tubular furnace is 550-650 ℃;
the sintering time is 3-7 h;
3. preheating and preparing a metal matrix:
placing the glass beads with the double-wall core-shell structure, which are coated by the C obtained in the step two, in a mold, directly compacting by utilizing the gravity of the powder, and then moving the powder into a heating furnace for preheating to obtain a preheated prefabricated body; heating the aluminum ingot weighed in the step one to 250-450 ℃ above the melting point under the protective atmosphere to obtain a molten metal matrix;
4. liquid metal infiltration:
and (4) placing the preheated preform belt mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the preform in the mold, and performing pressure infiltration.
The embodiment has the following beneficial effects:
1. the method adopts a chemical method to coat the surfaces of the glass beads, and forms polymer-shaped gel when a high-concentration alkaline catalyst is used, namely the obtained gel is formed by tightly connecting small particles, the connection area among the particles is large, the gel has high specific surface area and high mechanical strength, the floating part in the solution after the treatment process ensures that the glass beads are complete, and the chemical treatment process can realize uniform and continuous coating on the surfaces of the glass beads.
2. The thickness of the coated C shell can be regulated and controlled by changing the PH value of the solution and the content of the reactant, and the C shells with different coating thicknesses can be designed according to requirements.
3. The strength of the glass bead Al porous composite material with the core-shell structure prepared by the embodiment is obviously improved, wherein the peak stress is up to 190.2MPa,the highest energy absorption capacity reaches 83.2MJ/cm 3 。
4. The embodiment adopts gravity compaction, and the preform is prepared without pressurization, so that the integrity of the glass beads is ensured as much as possible in the preparation process of the preform, and the integrity of the glass beads is ensured as much as possible.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the average grain diameter of the glass microballoons in the first step is 18-60 mu m, and the ratio of the wall thickness to the radius is (0.043-0.064): 1.
the third concrete implementation mode: the first or second difference between the present embodiment and the specific embodiment is: the mass fraction of the alcohol in the step one is 98%.
The fourth concrete implementation mode is as follows: the difference between this embodiment mode and one of the first to third embodiment modes is: the stirring time in the second step is 6-30 h.
The fifth concrete implementation mode is as follows: the difference between this embodiment and one of the first to fourth embodiments is: the vacuum drying time in the second step is 6-24 h, and the temperature is 80-120 ℃.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: and the protective atmosphere in the second step and the third step is nitrogen, helium or argon.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the preheating process comprises the following steps: heating from room temperature to 50-100 ℃ below the melting point of the aluminum ingot in the mixed powder, and keeping the temperature for 4-8 h.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: step four, the pressure infiltration process comprises the following steps: the pressure is 5-10 MPa, the infiltration speed is 0.5-1 mm/s, the molten metal is completely infiltrated into the glass beads, the glass beads are cooled to the room temperature, and finally the die is removed.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and step four, the cooling speed is 10-20 ℃/min.
The detailed implementation mode is ten: the present embodiment differs from the ninth embodiment in that: and step four, the cooling speed is 15 ℃/min.
Example 1:
the preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material comprises the following steps:
1. weighing;
weighing glass beads and 40% of aluminum ingot according to the volume fraction of 60%; weighing appropriate amount of alcohol, deionized water, ammonia water, formaldehyde and resorcinol, and mixing to obtain a solution;
the average grain diameter of the glass beads is 40 mu m, and the wall thickness radius ratio is 0.064;
the volume ratio of the alcohol to the deionized water to the ammonia water to the formaldehyde is 350;
the mass ratio of the resorcinol to the formaldehyde is 1g:1.4mL; the mass of the resorcinol is 2g;
the mass fraction of the alcohol is 98 percent;
2. preparing glass beads with a C-coated double-wall core-shell structure;
placing glass beads in the solution prepared in the first step, stirring for 12 hours by using a magnetic stirrer, taking out solid floating in the liquid, drying in a vacuum drying oven, and sintering the dried powder in a tube furnace under a protective atmosphere to obtain C-coated glass beads with a double-wall core-shell structure;
the mass ratio of the glass beads to the volume of the solution prepared in the first step is 1g;
the stirring time is 12 hours;
the vacuum drying time is 6h, and the temperature is 80 ℃;
the protective atmosphere is nitrogen;
the sintering temperature of the tubular furnace is 600 ℃;
the sintering time is 5h;
3. preheating and preparing a metal matrix:
placing the glass beads with the double-wall core-shell structure coated by C obtained in the step two into a mold, directly compacting by using the gravity of the powder, and then moving the powder into a heating furnace for preheating to obtain a preheated prefabricated body; heating the aluminum ingot weighed in the step one to 300 ℃ above the melting point under the protection atmosphere of nitrogen to obtain a molten metal matrix; the aluminum ingot is made of Al-Si alloy, and the melting point is 640 ℃;
the preheating process comprises the following steps: heating from room temperature to 50 ℃ below the melting point of the aluminum ingot in the mixed powder and preserving heat for 4 hours;
4. liquid metal infiltration:
placing the preheated preform with the mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the preform in the mold, and performing pressure infiltration;
the pressure infiltration process comprises the following steps: the pressure is 5MPa, the infiltration speed is 0.5mm/s, molten metal is completely infiltrated into the glass beads, the glass beads are cooled to room temperature, and finally the mold is removed;
the cooling rate was 10 ℃/min.
FIG. 1 is an SEM photograph of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material obtained in example 1. As can be seen, no significant voids were observed in the composite. Through detection, the peak stress of the composite material is 123.7MPa, the platform stress is 110MPa, and the energy absorption capacity is 54.6MJ/cm 3 。
Example 2:
the preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material comprises the following steps:
1. weighing;
weighing glass beads and 40% of aluminum ingots according to the volume fraction of 60%; weighing appropriate amount of alcohol, deionized water, ammonia water, formaldehyde and resorcinol, and mixing to obtain a solution;
the average grain diameter of the glass beads is 20 microns, and the wall thickness radius ratio is 0.064;
the volume ratio of the alcohol to the deionized water to the ammonia water to the formaldehyde is 350; the mass fraction of the alcohol is 98 percent;
the mass ratio of the resorcinol to the formaldehyde is 1g:1.4mL; the mass of the resorcinol is 2g;
2. preparing glass beads with a C-coated double-wall core-shell structure;
placing glass beads in the solution prepared in the first step, stirring for 12 hours by using a magnetic stirrer, taking out solid floating in the liquid, drying in a vacuum drying oven, and sintering the dried powder in a tube furnace under a protective atmosphere to obtain C-coated glass beads with a double-wall core-shell structure;
the mass of the glass beads and the volume ratio of the solution prepared in the first step are 1 g;
the stirring time is 24 hours;
the vacuum drying time is 12h, and the temperature is 100 ℃;
the protective atmosphere is argon;
the sintering temperature of the tubular furnace is 600 ℃;
the sintering time is 6h;
3. preheating and preparing a metal matrix:
placing the glass beads with the double-wall core-shell structure, which are coated by the C obtained in the step two, in a mold, directly compacting by utilizing the gravity of the powder, and then moving the powder into a heating furnace for preheating to obtain a preheated prefabricated body; heating the aluminum ingot weighed in the step one to 300 ℃ above the melting point under the protection atmosphere of nitrogen to obtain a molten metal matrix; the aluminum ingot is made of Al-Si alloy, and the melting point is 640 ℃;
the preheating process comprises the following steps: heating from room temperature to 100 ℃ below the melting point of the metal powder in the mixed powder and keeping the temperature for 6 hours;
4. liquid metal infiltration:
placing the preheated preform with the mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the preform in the mold, and performing pressure infiltration;
the pressure infiltration process comprises the following steps: the pressure is 8MPa, the impregnating speed is 1mm/s, molten metal is completely impregnated into the glass beads, the glass beads are cooled to room temperature, and finally the die is removed;
the cooling rate was 10 ℃/min.
The detection proves that the peak stress of the composite material is 180.1MPa, the platform stress is 166.3MPa, and the energy absorption capacity is 80.2MJ/cm 3 。
Example 3:
the preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material comprises the following steps:
1. weighing;
weighing glass beads and 40% of aluminum ingots according to the volume fraction of 60%; weighing appropriate amount of alcohol, deionized water, ammonia water, formaldehyde and resorcinol, and mixing to obtain a solution;
the average grain diameter of the glass beads is 18 mu m, and the wall thickness radius ratio is 0.064;
the volume ratio of the alcohol to the deionized water to the ammonia water to the formaldehyde is 350;
the mass fraction of the alcohol is 98 percent;
the mass ratio of the resorcinol to the formaldehyde is 1.4g:2mL; the mass of the resorcinol is 4g;
2. c, preparing glass beads with a coated double-wall core-shell structure;
placing glass beads in the solution prepared in the first step, stirring for 12 hours by using a magnetic stirrer, taking out floating solids in the liquid, drying in a vacuum drying oven, and sintering the dried powder in a tube furnace under a protective atmosphere to obtain C-coated glass beads with a double-wall core-shell structure;
the volume ratio of the mass of the glass microspheres to the volume of the solution prepared in the first step is 1g;
the stirring time is 30h;
the vacuum drying time is 24 hours, and the temperature is 100 ℃;
the protective atmosphere is nitrogen;
the sintering temperature of the tubular furnace is 650 ℃;
the sintering time is 7h;
3. preheating and preparing a metal matrix:
placing the glass beads with the double-wall core-shell structure, which are coated by the C obtained in the step two, in a mold, directly compacting by utilizing the gravity of the powder, and then moving the powder into a heating furnace for preheating to obtain a preheated prefabricated body; heating the aluminum ingot weighed in the step one to 450 ℃ above the melting point under the protection atmosphere of nitrogen to obtain a molten metal matrix; the aluminum ingot is made of Al-Si alloy, and the melting point is 640 ℃;
the preheating process comprises the following steps: heating from room temperature to 50 ℃ below the melting point of the metal powder in the mixed powder and keeping the temperature for 8 hours;
4. liquid metal infiltration:
placing the preheated preform belt mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the preform in the mold, and performing pressure infiltration;
the pressure infiltration process comprises the following steps: the pressure is 10MPa, the impregnating speed is 1mm/s, molten metal is completely impregnated into the glass beads, the glass beads are cooled to room temperature, and finally the die is removed;
the cooling rate was 20 ℃/min.
Through detection, the peak stress of the composite material is 190.2MPa, the platform stress is 170.3MPa, and the energy absorption capacity is 83.2MJ/cm 3 。
Claims (10)
1. A preparation method of a high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material is characterized by comprising the following steps: the preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material comprises the following steps:
1. weighing;
weighing glass microspheres and the balance of aluminum ingots according to the volume fraction of 40 to 60 percent; weighing appropriate amount of alcohol, deionized water, ammonia water, formaldehyde and resorcinol, and mixing to obtain a solution;
the volume ratio of the alcohol to the deionized water to the ammonia water to the formaldehyde is 350 (15 to 45) to (2.8 to 5.6);
the mass ratio of the resorcinol to the formaldehyde is 1g: (1 to 2) mL;
2. c, preparing glass beads with a coated double-wall core-shell structure;
placing glass beads in the solution prepared in the first step, stirring for 12 hours by using a magnetic stirrer, taking out the glass beads floating in the liquid, drying in a vacuum drying oven, and sintering the dried powder in a tube furnace under a protective atmosphere to obtain C-coated glass beads with a double-wall core-shell structure;
the mass of the glass microspheres and the volume ratio of the solution prepared in the first step are 1g (10-50) mL;
the sintering temperature of the tube furnace is 550-650 ℃;
the sintering time is 3 to 7h;
3. preheating and preparing a metal matrix:
placing the glass beads with the double-wall core-shell structure, which are coated by the C obtained in the step two, in a mold, directly compacting by utilizing the gravity of the powder, and then moving the powder into a heating furnace for preheating to obtain a preheated prefabricated body; heating the aluminum ingot weighed in the step one to the temperature of 250-450 ℃ above the melting point under a protective atmosphere to obtain a molten metal matrix;
4. liquid metal infiltration:
and (4) placing the preheated preform with the mold obtained in the third step on the table top of a press machine, pouring the molten metal matrix on the preform in the mold, and performing pressure infiltration.
2. The preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material according to claim 1, which is characterized by comprising the following steps: the average grain diameter of the glass microspheres in the first step is 18 to 60 micrometers, and the wall thickness and the radius ratio are (0.043 to 0.064): 1.
3. the preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material according to claim 1, characterized by comprising the following steps: the mass fraction of the alcohol in the step one is 98%.
4. The preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material according to claim 1, which is characterized by comprising the following steps: and the stirring time in the second step is 6 to 30h.
5. The preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material according to claim 1, which is characterized by comprising the following steps: and the vacuum drying time of the step two is 6 to 24h, and the temperature is 80 to 120 ℃.
6. The preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material according to claim 1, which is characterized by comprising the following steps: and the protective atmosphere in the second step and the third step is nitrogen, helium or argon.
7. The preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material according to claim 1, which is characterized by comprising the following steps: the preheating process in the third step comprises the following steps: heating the mixture from room temperature to 50 to 100 ℃ below the melting point of an aluminum ingot in the mixed powder, and keeping the temperature for 4 to 8 hours.
8. The preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material according to claim 1, characterized by comprising the following steps: the pressure infiltration process comprises the following steps: the pressure is 5 to 10MPa, the impregnation speed is 0.5 to 1mm/s, the molten metal is completely impregnated into the glass microspheres, the temperature is cooled to the room temperature, and finally the mold is released.
9. The preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material according to claim 1, characterized by comprising the following steps: and the cooling speed in the fourth step is 10 to 20 ℃/min.
10. The preparation method of the high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material according to claim 9, characterized by comprising the following steps: and step four, the cooling speed is 15 ℃/min.
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