CN112207279A - Preparation method of bicontinuous magnesium-based composite material - Google Patents
Preparation method of bicontinuous magnesium-based composite material Download PDFInfo
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- CN112207279A CN112207279A CN202011143145.9A CN202011143145A CN112207279A CN 112207279 A CN112207279 A CN 112207279A CN 202011143145 A CN202011143145 A CN 202011143145A CN 112207279 A CN112207279 A CN 112207279A
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- magnesium
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- composite material
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 239000011777 magnesium Substances 0.000 title claims abstract description 34
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 109
- 238000005245 sintering Methods 0.000 claims abstract description 51
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 41
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 30
- 239000006260 foam Substances 0.000 claims abstract description 17
- 238000005498 polishing Methods 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 229910000990 Ni alloy Inorganic materials 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000010355 oscillation Effects 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 4
- 230000002787 reinforcement Effects 0.000 abstract description 18
- 239000011159 matrix material Substances 0.000 abstract description 16
- 238000002490 spark plasma sintering Methods 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 230000006835 compression Effects 0.000 description 7
- 238000007906 compression Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000003723 Smelting Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 238000005728 strengthening Methods 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000013016 damping Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- -1 whiskers Substances 0.000 description 1
Images
Classifications
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
Abstract
The invention discloses a preparation method of a bicontinuous magnesium-based composite material, and belongs to the technical field of composite material preparation. In the bicontinuous magnesium-based composite material, a matrix is magnesium alloy powder or pure magnesium powder, and a reinforcement is foamed nickel; the preparation method comprises the following steps: firstly, pretreating magnesium alloy powder or pure magnesium powder and foamed nickel, carrying out vacuum drying and ball milling treatment on the magnesium alloy powder or pure magnesium powder, and carrying out electrochemical polishing on the foamed nickel; sequentially placing the pretreated foam nickel and magnesium alloy powder into a sintering mold, and sintering in a Spark Plasma Sintering (SPS) technology to obtain the bicontinuous magnesium-based composite material with high density and excellent performance; compared with magnesium alloy or pure magnesium under the same sintering condition, the mechanical property of the composite material is obviously improved.
Description
Technical Field
The invention relates to a preparation method of a bicontinuous magnesium-based composite material, belonging to the technical field of alloy material preparation.
Background
Magnesium and its alloy have the advantages of low density, high specific strength and specific modulus, excellent damping and shock-absorbing performance, etc., and thus are one of the most promising materials in the modern high-tech field. However, the poor mechanical properties of magnesium alloy severely limit the application of magnesium alloy in modern engineering field. At present, the method capable of effectively enhancing the mechanical property of the magnesium alloy is to compound the magnesium alloy. The most important to the composite is the choice of reinforcement and the manufacturing process, typical reinforcements include mainly particles, whiskers, fibers, etc. The uniformity of the distribution of these reinforcements in the matrix has always been an unavoidable problem in composite materials, which affects the final mechanical properties of the material and causes local stress concentrations in the matrix when external forces are applied, due to the discontinuous distribution of the reinforcements in the matrix. The method for preparing the magnesium-based composite material mainly comprises smelting and powder metallurgy, wherein the smelting method has the problems of easy oxidation, limited components, coarse grains, more defects, unsatisfactory formability and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a bicontinuous magnesium-based composite material, wherein a reinforcement in the composite material is a continuous reinforcement, the structural integrity and continuity of the continuous reinforcement can form effective load transfer, the structure can also promote the realization of good damping capacity and enhanced damage tolerance, and the mechanical properties of magnesium and magnesium alloy can be effectively and further improved, and the method specifically comprises the following steps:
(1) pretreating magnesium alloy powder (or pure magnesium powder) and foamed nickel, carrying out vacuum drying and ball milling treatment on the magnesium alloy powder (or pure magnesium powder), carrying out electrochemical polishing on the foamed nickel, and then putting the foamed nickel into alcohol for ultrasonic oscillation.
(2) And sequentially putting the pretreated foam nickel and magnesium alloy powder (or pure magnesium powder) into a sintering mold, and applying a pre-pressure of about 15MPa to compact the powder and the foam nickel.
(3) And (3) placing the sintering mold into an SPS sintering cavity, fixing a thermocouple, ensuring that the load applied in the sintering process is parallel to the axial direction of the mold so as to ensure that bias voltage cannot be caused in the sintering and pressure applying process to damage the mold, and starting to electrify and apply pressure to sinter when the vacuum degree reaches below 12 Pa.
(4) And after sintering is finished, demolding the sintered sample by using a press machine when the temperature of the die is reduced to 100-130 ℃.
Preferably, the particle size of the magnesium alloy powder (or pure magnesium powder) is 400 meshes; the purity of the foamed nickel is more than or equal to 99.9 percent, the aperture is 0.1-3 mm, and the volume density is 0.2-1.5 g/cm3The magnesium alloy powder (or pure magnesium powder) is added in an amount to fill the voids of the nickel foam.
Preferably, the conditions for electrochemical polishing in step (1) of the present invention are: 15% nital solution, voltage 10V, polishing time 40 s.
Preferably, the sintering conditions in step (3) of the present invention are: continuously applying axial pressure of 30-35 MPa and sintering temperature of 440-580 ℃, and then keeping the temperature for 10-30 min at the sintering temperature.
The invention has the beneficial effects that:
(1) compared with pure magnesium alloy, the compressive strength and the compression ratio of the bicontinuous magnesium-based composite material are respectively improved by 6-19% and 14-30.7%, the foamed nickel serves as a framework support in the matrix and has a constraint effect on powder particles, and meanwhile, the foamed nickel and the matrix are subjected to element diffusion and reaction combination (2 Mg + Ni → Mg) in the sintering process2Ni) has an effect of strengthening the interface bonding between the reinforcement and the matrix, is less likely to cause stress concentration and cracks, and achieves an effect of load transfer.
(2) Compared with the traditional smelting process, the method provided by the invention has the advantages that the powder metallurgy technology can prepare the material with fine structure and excellent performance at a lower temperature, the problems of smelting, casting and other technologies can be effectively avoided, the material close to full compactness can be quickly prepared by utilizing the advantages of the SPS sintering technology, and the production efficiency is further improved.
Drawings
FIG. 1 is a schematic structural diagram of nickel foam;
FIG. 2 is a photograph of the surface of a bicontinuous ZK61/Ni composite prepared in example 1;
FIG. 3 is the microstructure of the bicontinuous ZK61/Ni composite of example 1;
FIG. 4 is a comparison of the compressibility of the bicontinuous ZK61/Ni composite of example 1 versus pure ZK61 alloy;
FIG. 5 is a fracture morphology of the bicontinuous ZK61/Ni composite of example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to the examples.
Example 1
A preparation method of a bicontinuous magnesium-based composite material specifically comprises the following steps:
(1) pretreating ZK61 magnesium alloy powder and foamed nickel, carrying out vacuum drying and ball milling treatment on the ZK61 magnesium alloy powder for 2 hours, and carrying out electrochemical polishing on the foamed nickel, wherein the conditions of the electrochemical polishing are as follows: 15% nitric acid alcohol solution, the voltage is 10V, and the polishing time is 40 s; then putting the mixture into alcohol for ultrasonic oscillation; the granularity of the magnesium alloy powder (or pure magnesium powder) is 400 meshes; the purity of the foamed nickel is more than or equal to 99.9 percent, the aperture is 1.27mm, and the volume density is 0.3g/cm3。
(2) And sequentially putting the pretreated foamed nickel and ZK61 magnesium alloy powder into a sintering die, and applying a pre-pressure of about 15MPa to compact the powder and the foamed nickel.
(3) The sintering mold is arranged in the SPS sintering cavity, a thermocouple is fixed, and the load applied in the sintering process is ensured to be parallel to the axial direction of the mold so as to ensure that bias voltage cannot be caused in the sintering and pressing process to damage the mold; when the vacuum degree reaches below 12Pa, electrifying and pressurizing for sintering; continuously applying axial pressure of 35MPa, heating to 400 ℃ at a speed of 50 ℃/min in the sintering process, heating to 440 ℃ at a speed of 20 ℃/min, finally heating to 500 ℃ at a speed of 15 ℃/min, and keeping the temperature for 10 min.
(4) After sintering, when the temperature of the mold is reduced to about 120 ℃, demolding the sintered sample by using a press machine to obtain the bicontinuous magnesium-based composite material, as shown in figure 2.
The obtained bicontinuous ZK61/Ni composite material is compared with the mechanical properties of a ZK61 magnesium alloy under the same sintering condition, the compressive strength and the compression ratio of the bicontinuous ZK61/Ni composite material are 371MPa and 17.0% respectively, the compressive strength and the compression ratio of a pure ZK61 magnesium alloy are 350MPa and 13.0% respectively, and the addition of continuous reinforcement foam nickel leads to the remarkable improvement of the overall mechanical properties of the ZK61 magnesium alloy.
In addition, the nickel foam and the matrix are subjected to element diffusion and reaction bonding in the sintering process (2 Mg + Ni → Mg)2Ni) having an effect of strengthening the interface bonding between the reinforcement and the matrix, as shown in fig. 3; observing the fracture morphology of the bicontinuous ZK61/Ni composite material, finding that the combination effect of the foam nickel of the reinforcement and the matrix is good, and no crack appears, as shown in FIG. 5; meanwhile, the material prepared by spark plasma sintering has higher density, and the density of all samples is more than 99%.
Example 2
A preparation method of a bicontinuous magnesium-based composite material specifically comprises the following steps:
(1) pretreating AZ91 magnesium alloy powder and foamed nickel, carrying out vacuum drying and ball milling treatment on the AZ91 magnesium alloy powder for 2h, and carrying out electrochemical polishing on the foamed nickel, wherein the conditions of the electrochemical polishing are as follows: 15% nitric acid alcohol solution, the voltage is 10V, and the polishing time is 40 s; then putting the magnesium alloy powder into alcohol for ultrasonic oscillation, wherein the granularity of the magnesium alloy powder (or pure magnesium powder) is 400 meshes; the purity of the foamed nickel is more than or equal to 99.9 percent, the aperture is 0.5mm, and the volume density is 1.5g/cm3。
(2) And sequentially putting the pretreated foamed nickel and AZ91 magnesium alloy powder into a sintering die, and applying a pre-pressure of about 15MPa to compact the powder and the foamed nickel.
(3) The sintering mold is arranged in the SPS sintering cavity, a thermocouple is fixed, and the load applied in the sintering process is ensured to be parallel to the axial direction of the mold so as to ensure that bias voltage cannot be caused in the sintering and pressing process to damage the mold; when the vacuum degree reaches below 12Pa, electrifying and pressurizing for sintering; continuously applying axial pressure of 30MPa, heating to 440 ℃ at 50 ℃/min in the sintering process, heating to 550 ℃ at 20 ℃/min, finally heating to 580 ℃ at 15 ℃/min, and keeping the temperature for 10 min.
(4) And after sintering is finished, demolding the sintered sample by using a press machine when the temperature of the die is reduced to about 120 ℃.
The mechanical properties of the obtained bicontinuous AZ91/Ni composite material are compared with those of AZ91 magnesium alloy under the same sintering condition, the compressive strength and the compression ratio of the bicontinuous AZ91/Ni composite material are 365MPa and 14 percent respectively, the compressive strength and the compression ratio of pure AZ91 magnesium alloy are 326MPa and 11 percent respectively, and the addition of continuous reinforcement foam nickel leads to the remarkable improvement of the overall mechanical properties of the AZ91 magnesium alloy.
In addition, the nickel foam and the matrix are subjected to element diffusion and reaction bonding in the sintering process (2 Mg + Ni → Mg)2Ni) has the effect of strengthening the interface combination between the reinforcement and the matrix, and the fracture morphology of the bicontinuous AZ91/Ni composite material is observed, so that the combination effect of the foam nickel of the reinforcement and the matrix is good, and no crack appears; meanwhile, the material prepared by spark plasma sintering has higher density, and the density of all samples is more than 99%.
Example 3
A preparation method of a bicontinuous magnesium-based composite material specifically comprises the following steps:
(1) pretreating pure magnesium powder and foamed nickel, carrying out vacuum drying and ball milling treatment on the pure magnesium powder for 2 hours, and carrying out electrochemical polishing on the foamed nickel, wherein the conditions of the electrochemical polishing are as follows: 15% nitric acid alcohol solution, the voltage is 10V, and the polishing time is 40 s; then putting the magnesium alloy powder into alcohol for ultrasonic oscillation, wherein the granularity of the magnesium alloy powder (or pure magnesium powder) is 400 meshes; the purity of the foamed nickel is more than or equal to 99.9 percent, the aperture is 3mm, and the volume density is 0.5g/cm3。
(2) And sequentially putting the pretreated foam nickel and pure magnesium powder into a sintering die, and applying a pre-pressure of about 15MPa to compact the powder and the foam nickel.
(3) The sintering mold is arranged in the SPS sintering cavity, a thermocouple is fixed, and the load applied in the sintering process is ensured to be parallel to the axial direction of the mold so as to ensure that bias voltage cannot be caused in the sintering and pressing process to damage the mold; when the vacuum degree reaches below 12Pa, electrifying and pressurizing for sintering; continuously applying axial pressure of 35MPa, heating to 480 ℃ at 60 ℃/min in the sintering process, heating to 540 ℃ at 30 ℃/min, finally heating to 580 ℃ at 20 ℃/min, and keeping the temperature for 15 min.
(4) And after sintering is finished, demolding the sintered sample by using a press machine when the temperature of the die is reduced to about 120 ℃.
The mechanical properties of the obtained bicontinuous Mg/Ni composite material are compared with those of pure magnesium under the same sintering condition, the compressive strength and the compression ratio of the bicontinuous Mg/Ni composite material are 257MPa and 32 percent respectively, the compressive strength and the compression ratio of the pure magnesium are 216MPa and 28 percent respectively, and the strength of the pure magnesium is obviously improved due to the addition of the continuous reinforcement foam nickel.
In addition, the nickel foam and the matrix are subjected to element diffusion and reaction bonding in the sintering process (2 Mg + Ni → Mg)2Ni) has the effect of strengthening the interface bonding between the reinforcement and the matrix, and the fracture morphology of the bicontinuous Mg/Ni composite material is observed, so that the reinforcement foamed nickel has good bonding effect with the matrix and no crack appears; meanwhile, the material prepared by spark plasma sintering has higher density, and the density of all samples is more than 99%.
Claims (4)
1. The preparation method of the bicontinuous magnesium-based composite material is characterized by comprising the following steps of:
(1) pretreating magnesium alloy powder/pure magnesium powder and foamed nickel, and carrying out vacuum drying and ball milling treatment on the magnesium alloy powder; performing electrochemical polishing on the foamed nickel, and then putting the foamed nickel into alcohol for ultrasonic oscillation;
(2) sequentially placing the pretreated foam nickel and magnesium alloy powder/pure magnesium powder into a sintering mold, and applying pre-pressure to compact the powder and the foam nickel;
(3) putting the sintering mold into an SPS sintering cavity, fixing a thermocouple, starting to electrify and applying pressure to sinter when the vacuum degree reaches below 12 Pa;
(4) and after sintering is finished, demolding the sintered sample by using a press machine when the temperature of the die is reduced to 100-130 ℃.
2. The process for the preparation of a bicontinuous magnesium-based composite material as claimed in claim 1, characterized in that: the granularity of the magnesium alloy powder or pure magnesium powder is 400 meshes, the purity of the foamed nickel is more than or equal to 99.9 percent, the aperture is 0.1-3 mm, and the volume density is 0.2-1.5 g/cm3。
3. The process for the preparation of a bicontinuous magnesium-based composite material as claimed in claim 1, characterized in that: the conditions of electrochemical polishing in the step (1) are as follows: 15% nital solution, voltage 10V, polishing time 40 s.
4. The process for the preparation of a bicontinuous magnesium-based composite material as claimed in claim 1, characterized in that: the sintering conditions in the step (3) are as follows: continuously applying axial pressure of 30-35 MPa and sintering temperature of 440-580 ℃, and then keeping the temperature for 10-30 min at the sintering temperature.
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| CN202011143145.9A CN112207279A (en) | 2020-10-23 | 2020-10-23 | Preparation method of bicontinuous magnesium-based composite material |
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| CN202011143145.9A CN112207279A (en) | 2020-10-23 | 2020-10-23 | Preparation method of bicontinuous magnesium-based composite material |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105543598A (en) * | 2016-03-01 | 2016-05-04 | 河北工业大学 | Preparation method of reinforced magnesium matrix composite |
| WO2017168126A1 (en) * | 2016-03-31 | 2017-10-05 | University Of Sunderland | Electrodes |
| CN107849642A (en) * | 2015-06-01 | 2018-03-27 | 耶达研究及发展有限公司 | Metal alloy composite |
| CN109909504A (en) * | 2019-02-28 | 2019-06-21 | 昆明理工大学 | A kind of porous foam enhancing metallic composite and preparation method thereof |
| KR20190080219A (en) * | 2017-12-28 | 2019-07-08 | (주)브이티엠 | Manufacturing composite material for marine cctv housing with excellent corrosion resistance and light weight and composite material for marine cctv housing manufactured thereby |
| 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 |
-
2020
- 2020-10-23 CN CN202011143145.9A patent/CN112207279A/en active Pending
Patent Citations (6)
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| CN107849642A (en) * | 2015-06-01 | 2018-03-27 | 耶达研究及发展有限公司 | Metal alloy composite |
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| WO2017168126A1 (en) * | 2016-03-31 | 2017-10-05 | University Of Sunderland | Electrodes |
| KR20190080219A (en) * | 2017-12-28 | 2019-07-08 | (주)브이티엠 | Manufacturing composite material for marine cctv housing with excellent corrosion resistance and light weight and composite material for marine cctv housing manufactured thereby |
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Application publication date: 20210112 |