CN115807176B - Preparation method of magnesium alloy combining spark plasma sintering and free fluid rapid cooling - Google Patents
Preparation method of magnesium alloy combining spark plasma sintering and free fluid rapid cooling Download PDFInfo
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- CN115807176B CN115807176B CN202211705861.0A CN202211705861A CN115807176B CN 115807176 B CN115807176 B CN 115807176B CN 202211705861 A CN202211705861 A CN 202211705861A CN 115807176 B CN115807176 B CN 115807176B
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Abstract
The invention relates to a preparation method of magnesium alloy by combining spark plasma sintering and free fluid rapid cooling, which aims at the problems of microstructure and performance. The preparation method has advanced process and accurate and real data, the prepared magnesium alloy has good metallographic structure compactness, no shrinkage cavity and shrinkage porosity defects, the grains in the metallographic structure show a small-to-large arrangement rule, and the average hardness is as high as 140.46HV, thus the preparation method is an advanced high-hardness magnesium alloy preparation method.
Description
Technical Field
The invention relates to a preparation method of a magnesium alloy by combining spark plasma sintering and free fluid rapid cooling, belonging to the technical field of nonferrous metal material preparation and application.
Background
With rapid development of aerospace, automobile industry and national defense and military fields and rapid consumption of petroleum resources of the earth, the demand for high-hardness light-weight metal components is increasing. The magnesium alloy has the characteristics of light weight, high specific stiffness, abrasion resistance, easy processing and recycling and the like, and is paid attention to by more and more researchers.
At present, the magnesium alloy castings produced by the conventional ingot metallurgy technology are easy to generate various defects, and the defects of loose, slag inclusion, cracks, air holes, coarse tissues and the like are common, so that the magnesium alloy produced by the conventional ingot metallurgy method has poor performances of compressive strength, high-temperature thermal stability, fracture toughness and the like.
Therefore, in order to improve the comprehensive properties of magnesium alloys, it is necessary to study new preparation processes.
Disclosure of Invention
Aiming at the defects of the background technology, the invention adopts a preparation method combining spark plasma sintering and free fluid rapid cooling to prepare the magnesium alloy so as to improve the mechanical property of the material.
The chemical materials used in the invention are as follows: magnesium powder, aluminum powder, zinc powder, manganese powder, silicon powder, copper powder and absolute ethyl alcohol, and the preparation dosage of the combination is as follows: in g/ml as unit of measurement
Magnesium powder: 50g + -1 g of Mg solid powder
Aluminum powder: 4.5g + -1 g of Al solid powder
Zinc powder: zn solid powder 0.3g + -0.1 g
Manganese powder: mn solid powder 0.1g + -0.01 g
Silicon powder: si solid powder 0.015g + -0.01 g
Copper powder: cu solid powder 0.01g + -0.001 g
Absolute ethyl alcohol: c (C) 2 H 5 OH liquid 500 mL.+ -. 50mL
The preparation method comprises the following steps:
1) Preparation work
Weighing 50 g+/-1 g magnesium powder, 4.5 g+/-1 g aluminum powder, 0.3 g+/-0.1 g zinc powder, 0.1 g+/-0.01 g manganese powder, 0.015 g+/-0.01 g silicon powder and 0.01 g+/-0.001 g copper powder, mixing all the powder, and pouring the mixture into an alcohol-containing ultrasonic cleaner for cleaning for at least 6min;
2) Mechanical stirring
Placing the cleaned powder into absolute ethyl alcohol for mechanical stirring, wherein the stirring speed is 350r/min, and the stirring time is 60min, so that the mechanical mixed powder is prepared;
3) Drying
Placing the mechanical mixed powder into a vacuum drying oven for drying, wherein the drying temperature is 60 ℃ and the drying time is 48 hours, so that the dried mechanical mixed powder is prepared;
4) Ball milling
(1) Adding the dried mechanical mixed powder into a ball milling tank of a planetary ball mill, wherein the volume ratio of the ball powder is 3:1;
(2) firstly, vacuumizing a ball milling tank, filling argon, and then performing ball milling for 100min to obtain magnesium alloy powder for strengthening alloying;
5) Pressurizing
(1) Placing the magnesium alloy powder for strengthening alloying into a graphite mold of a discharge plasma sintering furnace, and closing a furnace door after the mold is fixed;
(2) pumping out air in the furnace chamber by a vacuum pump: starting a vacuum pump, opening a vacuum valve to 5%, and opening the vacuum valve to 50% after the vacuum degree reaches below 0.06MPa, so that the vacuum degree reaches 3.3×10 rapidly -2 Pa；
(3) Opening an upper hydraulic station of a pressurizing device of the discharge plasma sintering furnace, and setting the pressurizing device of the discharge plasma sintering furnace: the pressure alarm value is set to 3.8T, and the actual pressure of the die is set to 3.6T;
(4) starting a pressurizing device of the discharge plasma sintering furnace to pressurize the magnesium alloy powder in the graphite mold, wherein the pressure is 50MPa;
6) Spark plasma sintering
(1) The process formula is set: setting the sintering heating rate to 20 ℃/min, setting the sintering temperature to 480 ℃ and setting the sintering time to 5min;
(2) the process is operated: starting a sintering device of the discharge plasma furnace, and sintering the magnesium alloy powder in the graphite mold;
7) Free fluid rapid cooling
(1) After the temperature is increased, under the action of continuous pressure, the magnesium alloy melt which is partially melted in the graphite mold is extruded from the liquid discharge hole and flows out freely along the graphite cushion block;
(2) after sintering is finished, the cooling water circulation device rapidly cools the graphite mold through a lower hydraulic station of a pressurizing device of the discharge plasma sintering furnace, so that the outflow magnesium alloy melt is rapidly solidified into a water drop-shaped magnesium alloy block;
8) Door of furnace
After cooling is finished, loosening four corner screws of the furnace door, closing the vacuumizing valve, closing the vacuum pump, opening the vacuum breaking valve, and bouncing the furnace door;
9) Cleaning and cleaning
Taking out the magnesium alloy block, and cleaning the surface of the magnesium alloy block;
10 Detection, analysis, characterization
Detecting, analyzing and characterizing the appearance, color, metallographic structure and mechanical property of the magnesium alloy block;
carrying out metallographic structure analysis by using a metallographic microscope;
hardness analysis was performed with a vickers hardness tester;
conclusion: the metallographic structure of the magnesium alloy has good compactness, no shrinkage cavity and shrinkage porosity defect, and the grains in the metallographic structure show a rule of arrangement from small to large, and the average hardness is as high as 140.46HV.
Compared with the background art, the invention has obvious advancement, and aims at the problems of microstructure and performance, adopts a preparation method combining spark plasma sintering and free fluid rapid cooling, prepares the magnesium alloy by mechanical stirring, drying, ball milling, pressurizing, spark plasma sintering and free fluid rapid cooling, and improves the mechanical property of the magnesium alloy. The preparation method has advanced process and accurate and real data, the prepared magnesium alloy has good metallographic structure compactness, no shrinkage cavity and shrinkage porosity defects, the grains in the metallographic structure show a small-to-large arrangement rule, and the average hardness is as high as 140.46HV, thus the preparation method is an advanced high-hardness magnesium alloy preparation method.
Drawings
Fig. 1 is a diagram of a combined spark plasma sintering and free fluid rapid cooling preparation state.
FIG. 2 is a diagram showing the microstructure morphology of the magnesium alloy prepared by the invention.
FIG. 3 is an enlarged partial microscopic morphology of the magnesium alloy produced according to the present invention.
FIG. 4 is a graph showing the hardness properties of magnesium alloys prepared according to the present invention.
The list of reference numerals shown in the figures is as follows:
the device comprises a 1-system control cabinet, a 2-display screen, a 3-control cabinet switch, a 4-temperature control knob, a 5-pressure control knob, a 6-time control knob, a 7-high frequency power switch, an 8-process formula setting knob, a 9-high frequency power negative electrode, a 10-negative electrode copper wire row, a 11-thermocouple, a 12-liquid discharge hole, a 13-circulating cooling water control cabinet, a 14-circulating cooling water switch, a 15-cooling fan switch, a 16-temperature measuring hole, a 17-water inlet, a 18-water outlet, an ascending button of a 19-upper hydraulic station, a descending button of a 20-upper hydraulic station, a 21-vacuum pump, a 22-lower hydraulic station, a 23-graphite gasket, a 24-vacuumizing valve, a 25-graphite cone, a 26-graphite cushion, a 27-discharge plasma sintering furnace graphite mold, a 28-magnesium alloy powder, a 29-vacuum breaking valve, a 30-vacuum meter, a 31-upper hydraulic station, a 32-positive electrode copper wire row, a 33-signal wire, a 34-alarm, a 35-high frequency power positive electrode, a 36-discharge plasma sintering furnace and a 37-liquid collecting tank.
Detailed Description
The invention is further described with reference to the accompanying drawings:
FIG. 1 is a diagram showing a combined preparation state of spark plasma sintering and free-fluid rapid cooling;
the whole set of equipment comprises a discharge plasma sintering furnace;
a vacuum breaking valve 29 and a vacuum gauge 30 are respectively arranged on a furnace body 36 of the discharge plasma sintering furnace;
the pressurizing device of the discharge plasma sintering furnace comprises an upper hydraulic station 31, a lower hydraulic station 22, two graphite gaskets 23, two graphite conical heads 25 and two graphite cushion blocks 26;
a liquid discharge hole 12 is arranged on a graphite mould 27 of the discharge plasma sintering furnace; a liquid collecting tank 37 is arranged right below the liquid discharging hole 12;
a graphite die 27, an upper hydraulic station 31 and a lower hydraulic station 22 of the discharge plasma sintering furnace are respectively provided with a temperature measuring hole 16; a thermocouple 11 is inserted into each of the three temperature measuring holes 16;
a cooling water circulation device is arranged below the furnace body 36 of the discharge plasma sintering furnace; the cooling water circulation device comprises a circulating cooling water control cabinet 13; the circulating cooling water control cabinet 13 is respectively provided with a circulating cooling water switch 14 and a cooling fan switch 15; the right side of the circulating cooling water control cabinet 13 is respectively provided with an ascending button 19 of an upper hydraulic station 31 and a descending button 20 of the upper hydraulic station 31; the lower hydraulic station 22 is respectively provided with a water inlet 17 and a water outlet 18; the water inlet 17 and the water outlet 18 are both communicated with the circulating cooling water control cabinet 13;
the right of the furnace body 36 of the discharge plasma sintering furnace is respectively provided with a vacuum pump 21 and a vacuumizing tube; the vacuum pump 21 is communicated with the furnace chamber of the discharge plasma sintering furnace through a vacuumizing tube; the vacuumizing tube is provided with a vacuumizing valve 24;
a system control cabinet 1 is arranged at the left side of a furnace body 36 of the discharge plasma sintering furnace; the system control cabinet 1 is respectively provided with a display screen 2, a control cabinet switch 3, a temperature control knob 4, a pressure control knob 5, a time control knob 6, a high-frequency power switch 7, a process formula setting knob 8 and an alarm 34; the system control cabinet 1 is connected with a pressurizing device of the discharge plasma sintering furnace through a signal line 33;
the sintering device of the discharge plasma sintering furnace comprises an anode copper wire row 32, a cathode copper wire row 10, a high-frequency power supply anode 35 and a high-frequency power supply cathode 9; one end of the positive copper wire row 32 is connected with the upper hydraulic station 31, and the other end is connected with the system control cabinet 1 through a high-frequency power supply positive electrode 35; one end of the negative copper wire row 10 is connected with a lower hydraulic station 22, and the other end is connected with the system control cabinet 1 through a high-frequency power negative electrode 9;
FIG. 2 shows a metallographic microstructure morphology diagram of the magnesium alloy prepared by the invention; as shown in the figure, the magnesium alloy prepared by the invention has good metallographic structure compactness, no shrinkage cavity and shrinkage porosity defects, and the grains in the metallographic structure show a rule of arrangement from small to large.
FIG. 3 shows a partially enlarged microscopic morphology of the magnesium alloy of the present invention, specifically, the morphology of the contact portion of the magnesium matrix with the second phase.
FIG. 4 is a graph showing the hardness properties of the magnesium alloy of the present invention; as shown in the figure, the average hardness of the magnesium alloy prepared by the invention is as high as 140.46HV.
While specific embodiments of the invention have been described above, it will be appreciated by those skilled in the art that these are by way of example only, and the scope of the invention is defined by the appended claims. Various changes and modifications to these embodiments may be made by those skilled in the art without departing from the principles and spirit of the invention, but such changes and modifications fall within the scope of the invention.
Claims (1)
1. A preparation method of a magnesium alloy combining spark plasma sintering and free fluid rapid cooling is characterized by comprising the following steps:
the chemical materials used are: magnesium powder, aluminum powder, zinc powder, manganese powder, silicon powder, copper powder and absolute ethyl alcohol, and the preparation dosage of the combination is as follows: in g/ml as unit of measurement
Magnesium powder: 50g + -1 g of Mg solid powder
Aluminum powder: 4.5g + -1 g of Al solid powder
Zinc powder: zn solid powder 0.3g + -0.1 g
Manganese powder: mn solid powder 0.1g + -0.01 g
Silicon powder: si solid powder 0.015g + -0.01 g
Copper powder: cu solid powder 0.01g + -0.001 g
Absolute ethyl alcohol: c (C) 2 H 5 OH liquid 500 mL.+ -. 50mL
The preparation method comprises the following steps:
1) Preparation work
Weighing 50 g+/-1 g magnesium powder, 4.5 g+/-1 g aluminum powder, 0.3 g+/-0.1 g zinc powder, 0.1 g+/-0.01 g manganese powder, 0.015 g+/-0.01 g silicon powder and 0.01 g+/-0.001 g copper powder, mixing all the powder, and pouring the mixture into an alcohol-containing ultrasonic cleaner for cleaning for at least 6min;
2) Mechanical stirring
Placing the cleaned powder into absolute ethyl alcohol for mechanical stirring, wherein the stirring speed is 350r/min, and the stirring time is 60min, so that the mechanical mixed powder is prepared;
3) Drying
Placing the mechanical mixed powder into a vacuum drying oven for drying, wherein the drying temperature is 60 ℃ and the drying time is 48 hours, so that the dried mechanical mixed powder is prepared;
4) Ball milling
(1) Adding the dried mechanical mixed powder into a ball milling tank of a planetary ball mill, wherein the volume ratio of the ball powder is 3:1;
(2) firstly, vacuumizing a ball milling tank, filling argon, and then performing ball milling for 100min to obtain magnesium alloy powder for strengthening alloying;
5) Pressurizing
(1) Placing the magnesium alloy powder for strengthening alloying into a graphite mold of a discharge plasma sintering furnace, and closing a furnace door after the mold is fixed;
(2) pumping out air in the furnace chamber by a vacuum pump: starting a vacuum pump, opening a vacuum valve to 5%, and opening the vacuum valve to 50% after the vacuum degree reaches below 0.06MPa, so that the vacuum degree reaches 3.3×10 rapidly -2 Pa；
(3) Opening an upper hydraulic station of a pressurizing device of the discharge plasma sintering furnace, and setting the pressurizing device of the discharge plasma sintering furnace: the pressure alarm value is set to 3.8T, and the actual pressure of the die is set to 3.6T;
(4) starting a pressurizing device of the discharge plasma sintering furnace to pressurize the magnesium alloy powder in the graphite mold, wherein the pressure is 50MPa;
6) Spark plasma sintering
(1) The process formula is set: setting the sintering heating rate to 20 ℃/min, setting the sintering temperature to 480 ℃ and setting the sintering time to 5min;
(2) the process is operated: starting a sintering device of the discharge plasma furnace, and sintering the magnesium alloy powder in the graphite mold;
7) Free fluid rapid cooling
(1) After the temperature is increased, under the action of continuous pressure, the magnesium alloy melt which is partially melted in the graphite mold is extruded from the liquid discharge hole and flows out freely along the graphite cushion block;
(2) after sintering is finished, the cooling water circulation device rapidly cools the graphite mold through a lower hydraulic station of a pressurizing device of the discharge plasma sintering furnace, so that the outflow magnesium alloy melt is rapidly solidified into a water drop-shaped magnesium alloy block;
8) Door of furnace
After cooling is finished, loosening four corner screws of the furnace door, closing the vacuumizing valve, closing the vacuum pump, opening the vacuum breaking valve, and bouncing the furnace door;
9) Cleaning and cleaning
Taking out the magnesium alloy block, and cleaning the surface of the magnesium alloy block;
10 Detection, analysis, characterization
Detecting, analyzing and characterizing the appearance, color, metallographic structure and mechanical property of the magnesium alloy block;
carrying out metallographic structure analysis by using a metallographic microscope;
hardness analysis was performed with a vickers hardness tester;
conclusion: the metallographic structure of the magnesium alloy has good compactness, no shrinkage cavity and shrinkage porosity defect, and the grains in the metallographic structure show a rule of arrangement from small to large, and the average hardness is as high as 140.46HV.
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| CN115807176B true CN115807176B (en) | 2023-08-11 |
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Citations (6)
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|---|---|---|---|---|
| WO2006006379A1 (en) * | 2004-07-08 | 2006-01-19 | Toudai Tlo, Ltd. | Magnesium-base composite powder, magnesium-base alloy material and method for production thereof |
| JP2013170284A (en) * | 2012-02-20 | 2013-09-02 | Nihon Univ | High-specific-strength magnesium exhibiting age hardening characteristic |
| CN104174849A (en) * | 2014-07-29 | 2014-12-03 | 太原理工大学 | Preparation method of fine-grain magnesium alloy block |
| JP2016194095A (en) * | 2015-03-31 | 2016-11-17 | 国立大学法人東北大学 | Method for manufacturing magnesium and iron alloy, magnesium and iron alloy, and organism medical material using the same |
| CN110273092A (en) * | 2019-08-01 | 2019-09-24 | 重庆大学 | A kind of CoCrNi particle reinforced magnesium base compound material and preparation method thereof |
| CN113151705A (en) * | 2021-04-08 | 2021-07-23 | 青海大学 | ZK60 magnesium alloy preparation method based on SPS technology |
-
2022
- 2022-12-29 CN CN202211705861.0A patent/CN115807176B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006006379A1 (en) * | 2004-07-08 | 2006-01-19 | Toudai Tlo, Ltd. | Magnesium-base composite powder, magnesium-base alloy material and method for production thereof |
| JP2013170284A (en) * | 2012-02-20 | 2013-09-02 | Nihon Univ | High-specific-strength magnesium exhibiting age hardening characteristic |
| CN104174849A (en) * | 2014-07-29 | 2014-12-03 | 太原理工大学 | Preparation method of fine-grain magnesium alloy block |
| JP2016194095A (en) * | 2015-03-31 | 2016-11-17 | 国立大学法人東北大学 | Method for manufacturing magnesium and iron alloy, magnesium and iron alloy, and organism medical material using the same |
| CN110273092A (en) * | 2019-08-01 | 2019-09-24 | 重庆大学 | A kind of CoCrNi particle reinforced magnesium base compound material and preparation method thereof |
| CN113151705A (en) * | 2021-04-08 | 2021-07-23 | 青海大学 | ZK60 magnesium alloy preparation method based on SPS technology |
Non-Patent Citations (1)
| Title |
|---|
| 挤压铸造Mg-Zn-Y合金显微组织与力学性能的研究;吴金珂等;铸造;第64卷(第12期);第1258-1263页 * |
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