CN103451464A - Mg2Si enhanced Mg alloy composite material - Google Patents
Mg2Si enhanced Mg alloy composite material Download PDFInfo
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- CN103451464A CN103451464A CN2013103795951A CN201310379595A CN103451464A CN 103451464 A CN103451464 A CN 103451464A CN 2013103795951 A CN2013103795951 A CN 2013103795951A CN 201310379595 A CN201310379595 A CN 201310379595A CN 103451464 A CN103451464 A CN 103451464A
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 22
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 229910019752 Mg2Si Inorganic materials 0.000 title abstract 3
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000007731 hot pressing Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 23
- 239000011777 magnesium Substances 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 17
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 15
- 238000001125 extrusion Methods 0.000 claims description 14
- 239000011159 matrix material Substances 0.000 claims description 13
- 230000001681 protective effect Effects 0.000 claims description 13
- 238000009413 insulation Methods 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 11
- 239000011863 silicon-based powder Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000008188 pellet Substances 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- LLQHSBBZNDXTIV-UHFFFAOYSA-N 6-[5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-4,5-dihydro-1,2-oxazol-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC1CC(=NO1)C1=CC2=C(NC(O2)=O)C=C1 LLQHSBBZNDXTIV-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 238000009768 microwave sintering Methods 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
- 230000005855 radiation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Abstract
The invention discloses an Mg2Si enhanced Mg alloy composite material. The Mg2Si enhanced Mg alloy composite material with excellent property is obtained by optimizing raw material ratios and technological parameters of high-temperature hot-pressing sintering in combination with corresponding pretreatment and aftertreatment. The relative density of the composite material is at least 98.5%, the tensile strength is at least 470MPa, and the elongation percentage is at least 12%.
Description
Technical field
The present invention relates to the technical field of Mg alloy, particularly a kind of Mg
2the Mg alloy composite materials that Si strengthens.
Background technology
Magnesium and alloy thereof have specific tenacity, specific rigidity is high, damping property is good, electromagnetic shielding and the advantage such as capability of resistance to radiation is strong, its good machining property and easily the recovery feature of environmental protection in addition, magnesium and alloy thereof have all obtained application and research extremely widely in numerous industrial circles such as automobile, electronics, electrical equipment, traffic, aerospace and national defense and military, and being described as is the 3rd metalloid structured material emerging after iron and steel and aluminium alloy.Yet magnesium alloy in general mechanical property and corrosion resistance nature still lower, largely restricted its use category.
In order to improve the mechanical property of magnesium alloy, introduce reinforcement to prepare matrix material the most effective method beyond doubt in alloy substrate, for example in magnesium alloy, introduce the Mg with high-melting-point, high strength and high elastic coefficient
2thereby Si obtains Mg
2si strengthens the Mg alloy composite materials and just worldwide conducts extensive research.Wherein main preparation method comprises powder metallurgy, extrusion casting, liquid metal-stirring etc.And powder metallurgy is the earliest for the technique of magnesium alloy particles reinforced composite, simultaneously because powder metallurgy needn't be through the condition of high temperature preparation of fine melt, can avoid greatly the variety of issues such as scaling loss, oxidation of magnesium, therefore still as the preparation technology of main magnesium base composite material.
The research that current powder metallurgy prepares magnesium alloy particles reinforced composite technique mainly concentrates in the novel sintering technology such as discharge plasma sintering, microwave sintering, although these emerging technologies have the advantages such as sintering temperature is low, sintering velocity is fast, but its cost of investment is large, the suitability for industrialized production difficulty is high, by contrast, relatively less about less investment, research easy and simple to handle, traditional hot pressed sintering of being easy to suitability for industrialized production.
Summary of the invention
Purpose of the present invention is to provide the Mg of a kind of Rational Parameters, excellent performance
2si strengthens the preparation method of Mg alloy composite materials and the Mg made thereof
2the Mg alloy composite materials that Si strengthens.
Particularly, the present invention adopts following technical scheme:
A kind of Mg
2the Mg alloy composite materials that Si strengthens is characterized in that it is prepared by following methods:
One, batching: the atomic ratio of take is got pure magnesium powder and pure silicon powder as about 84-88:16-12 joins, the granularity of wherein said pure magnesium powder is about 50-60 μ m, and the granularity of pure silicon powder is about 80-100 μ m, under about 150-180 ℃ condition, powder is carried out to drying and processing standby;
Two, batch mixing: the raw material prepared is put into to ball-grinding machine, passing under the Ar protective atmosphere of 250ml/min, take the rotating speed of 500rpm, the condition that the pellet particle diameter is about 5-8:1 as 5mm, ball material mass ratio, fully the about 45-60min of admixture activation obtains nanometer grade powder;
Three, pressed compact: mixed raw material is placed in the compacting tool set of Ar protective atmosphere, after being warming up to about 220-250 ℃ with 30 ℃/min, with about 220-250 ℃, the pressure of 30-40MPa, powder being carried out to pressed compact and process about 40-50min and obtain blank;
Four, hot pressed sintering: blank is packed in the sintering mold of the Ar protective atmosphere that passes into 250ml/min, speed with 20 ℃/min under about 30-50MPa pressure is warming up to 450 ℃, under about 50-70MPa pressure, the speed with 2 ℃/min slowly is warming up to about 540-560 ℃ uniformly again, after the about 60-90min of heat-insulation pressure keeping, controlling speed of cooling is that after 2 ℃/min to the 400 ℃ about 20-30min of insulation, stove is chilled to 220 ℃, obtains sintered compact;
Five, extrusion process: sintered compact is placed in rapidly to the mould that is preheating to 250 ℃, implements 5 passage extrusion process of the extrusion ratio of about 5-8 with the speed of 2mm/s, finally obtain Mg
2si strengthens the Mg alloy composite materials.
The granularity that adopts pure magnesium powder is about 50-60 μ m, the granularity of pure silicon powder is about 80-100 μ m, sintering structure for the even mixing of trickle powder and final matrix material is all most important, and dries the interference that can better remove moisture and avoid other reactions in ensuing ball mill mixing process.
Proportioning raw materials has keying action for structure property and the choosing of preparation technology parameter of matrix material undoubtedly, mate the most excellent performance for obtaining, the application limits take atomic ratio and gets pure magnesium powder and pure silicon powder as about 84-88:16-12 joins, preferably, take atomic ratio gets pure magnesium powder and pure silicon powder as 86:14 joins.
Whether the parameter of ball mill mixing full and uniform and whether powder obtains fully activation plays an important role for mixing, mix and fully activation be the basis of next step pressed compact, sintering.
The parameter of pressed compact, sintering and extrusion process has determined tissue and the performance quality of final matrix material jointly:
Preferably, carry out pressed compact with 240 ℃, 35MPa and process 45min;
Preferably, the high temperature hot pressing sintering is that the speed with 20 ℃/min is warming up to 450 ℃ under 40MPa pressure, under 60MPa pressure, the speed with 2 ℃/min slowly is warming up to 550 ℃ uniformly again, after heat-insulation pressure keeping 80min, controlling speed of cooling is that after 2 ℃/min to 400 ℃ insulation 30min, stove is chilled to 220 ℃, obtains sintered compact;
In addition, preferred, in batch mixing, high temperature hot pressing sintering stage, pass into the H that is less than 15ml/min in protective atmosphere
2.
The invention has the advantages that: by reasonably optimizing proportioning raw materials, preparation process and corresponding processing parameter, utilize traditional hot pressing sintering method to obtain the Mg of excellent performance
2si strengthens the Mg alloy composite materials.
Embodiment
Embodiment 1.
A kind of Mg
2si strengthens the preparation method of Mg alloy composite materials, it is characterized in that:
One, batching: the atomic ratio of take is got pure magnesium powder and pure silicon powder as about 84:16 joins, the granularity of wherein said pure magnesium powder is 50 μ m, and the granularity of pure silicon powder is 100 μ m, under 160 ℃ of conditions, powder is carried out to drying and processing standby;
Two, batch mixing: the raw material prepared is put into to ball-grinding machine, passing under the Ar protective atmosphere of 250ml/min, take the rotating speed of 500rpm, the condition that the pellet particle diameter is about 7:1 as 5mm, ball material mass ratio, fully the about 50min of admixture activation obtains nanometer grade powder;
Three, pressed compact: mixed raw material is placed in the compacting tool set of Ar protective atmosphere, after being warming up to 220 ℃ with 30 ℃/min, with 220 ℃, the pressure of 30MPa, powder being carried out to pressed compact and process about 40min and obtain blank;
Four, hot pressed sintering: blank is packed in the sintering mold of the Ar protective atmosphere that passes into 250ml/min, speed with 20 ℃/min under 30MPa pressure is warming up to 450 ℃, under about 50MPa pressure, the speed with 2 ℃/min slowly is warming up to approximately 540 ℃ uniformly again, after the about 60min of heat-insulation pressure keeping, controlling speed of cooling is that after 2 ℃/min to 400 ℃ insulation 30min, stove is chilled to 220 ℃, obtains sintered compact;
Five, extrusion process: sintered compact is placed in rapidly to the mould that is preheating to 250 ℃, the speed of 2mm/s of take is implemented the 5 passage extrusion process that extrusion ratio is 6, obtains Mg
2si strengthens the Mg alloy composite materials.
Implement 2-3 and comparative example 1-2.
Basic identical with the parameter of embodiment 1, difference is mainly that the ratio of pure magnesium powder and pure silicon powder is that embodiment 2 is 88:12 for 86:14, embodiment 3, and comparative example 1 is 90:10, and comparative example 2 is 80:20.
Table 1
| No. | Mg：Si(at) | Tensile strength (MPa) | Unit elongation (%) |
| 1 | 84：16 | 475 | 12.2 |
| 2 | 86：14 | 469 | 16.4 |
| 3 | 88：12 | 446 | 18.1 |
| 1* | 90：10 | 411 | 19.0 |
| 2* | 80：20 | 480 | 7.8 |
Test result from table 1, the performance that magnesium silicon is compared to matrix material has material impact, the tensile strength of embodiment 1-3 and unit elongation have suitability preferably, and the too low strengthening effect that causes of silicone content is inadequate, and the too high meeting of silicone content causes the unit elongation deficiency.
Implement 4-5 and comparative example 3-4.
Basic identical with the parameter of embodiment 1, difference mainly is to have changed the parameter of pressed compact.
Table 2
| No. | Temperature (℃) | Pressure (MPa) | Time (min) | Tensile strength (MPa) | Unit elongation (%) | Relative density (%) |
| 1 | 220 | 30 | 40 | 475 | 12.2 | 98.6 |
| 4 | 240 | 35 | 45 | 480 | 12.9 | 99.3 |
| 5 | 250 | 40 | 50 | 476 | 13.4 | 99.2 |
| 3* | 260 | 50 | 50 | 479 | 12.5 | 99.2 |
| 4* | 210 | 25 | 45 | 460 | 9.8 | 96.5 |
Test result from table 2, the processing parameter of pressed compact has considerable influence for performance and the relative density of matrix material, embodiment has very high relative density, and tensile strength and unit elongation excellence, discontented unabridged version application requirement may cause meaningless the increasing or the obvious variation of performance of cost.
Implement 6-7 and comparative example 5-8.
The parameter of implementing 6-7 and comparative example 5-6 and embodiment 1 is basic identical, and difference mainly is to have changed the hot pressed sintering parameter, and comparative example 7 does not adopt the pre-step heated up, and the temperature rise rate that comparative example 8 is the 2nd section is 4 ℃/min.
Table 3
| No. | Temperature (℃) | Pressure (MPa) | Time (min) | Tensile strength (MPa) | Unit elongation (%) | The Si phase |
| 1 | 540 | 50 | 60 | 475 | 12.2 | Substantially without |
| 6 | 550 | 60 | 80 | 490 | 14.3 | Nothing |
| 7 | 560 | 70 | 90 | 482 | 13.4 | Nothing |
| 5* | 530 | 50 | 60 | 420 | 8.5 | Have |
| 6* | 580 | 60 | 80 | 468 | 11.7 | Nothing |
| 7* | 550 | 60 | 80 | 469 | 11.8 | Substantially without |
| 8* | 560 | 50 | 60 | 415 | 9.6 | Have |
From the test result of table 3, the intensification of sintering order, temperature rise rate, sintering temperature and pressure, have decisive influence for the quality of hot pressed sintering, and the pre-process heated up and temperature rise rate are for whether can fully forming Mg
2thereby Si has avoided silica flour not react and has participated in material impact.
Enforcement 8 and comparative example 9-10.
Embodiment 8 mainly is to pass in batch mixing, high temperature hot pressing sintering stage the H that is less than 15ml/min in protective atmosphere
2, comparative example 9 after heat-insulation pressure keeping directly stove be chilled to room temperature and do not carry out extrusion process, after comparative example 10 heat-insulation pressure keepings directly stove be chilled to 220 ℃, then be placed in preheated mold and carry out extrusion process.
Table 4
| No. | Tensile strength (MPa) | Unit elongation (%) | Relative density (%) |
| 1 | 475 | 12.2 | 98.6 |
| 8 | 482 | 19.1 | 99.4 |
| 9* | 375 | 15.6 | 90.2 |
| 10* | 422 | 10.0 | 97.5 |
From the test result of table 4, if, in batch mixing, high temperature hot pressing sintering stage, pass into the H that is less than 15ml/min in protective atmosphere
2, can effectively improve relative density and the mechanical property of matrix material.And, from the contrast of comparative example 9 and 10, the cooling performance for matrix material of temperature control after the few sintering of extrusion process and heat also has a great impact.
Claims (6)
1. a Mg
2the Mg alloy composite materials that Si strengthens is characterized in that described material prepares by the following method:
One, batching: the atomic ratio of take is got pure magnesium powder and pure silicon powder as 84-88:16-12 joins, the granularity of wherein said pure magnesium powder is 50-60 μ m, and the granularity of pure silicon powder is 80-100 μ m, under 150-180 ℃ of condition, powder is carried out to drying and processing standby;
Two, batch mixing: the raw material prepared is put into to ball-grinding machine, passing under the Ar protective atmosphere of 250ml/min, take the rotating speed of 500rpm, the condition that the pellet particle diameter is 5-8:1 as 5mm, ball material mass ratio, fully admixture activation 45-60min obtains nanometer grade powder;
Three, pressed compact: mixed raw material is placed in the compacting tool set of Ar protective atmosphere, with 220-250 ℃, the pressure of 30-40MPa, powder is carried out to pressed compact and process 40-50min and obtain blank;
Four, hot pressed sintering: blank is packed in the sintering mold of the Ar protective atmosphere that passes into 250ml/min, speed with 20 ℃/min under 30-50MPa pressure is warming up to 450 ℃, under 50-70MPa pressure, the speed with 2 ℃/min slowly is warming up to 540-560 uniformly again, after heat-insulation pressure keeping 60-90min, controlling speed of cooling is that after 2 ℃/min to 400 ℃ insulation 20-30min, stove is chilled to 220 ℃, obtains sintered compact;
Five, extrusion process: sintered compact is placed in rapidly to the mould that is preheating to 250 ℃, implements 5 passage extrusion process of the extrusion ratio of 5-8 with the speed of 2mm/s, finally obtain Mg
2si strengthens the Mg alloy composite materials.
2. matrix material according to claim 1, it is characterized in that: the atomic ratio of take is got pure magnesium powder and pure silicon powder as 86:14 joins.
3. matrix material according to claim 1 is characterized in that: with 240 ℃, 35MPa, carry out pressed compact and process 45min.
4. matrix material according to claim 1, it is characterized in that: the high temperature hot pressing sintering is that the speed with 20 ℃/min is warming up to 450 ℃ under 40MPa pressure, under 60MPa pressure, the speed with 2 ℃/min slowly is warming up to 550 uniformly again, after heat-insulation pressure keeping 80min, controlling speed of cooling is that after 2 ℃/min to 400 ℃ insulation 30min, stove is chilled to 220 ℃, obtains sintered compact.
5. matrix material according to claim 1, is characterized in that: in batch mixing, high temperature hot pressing sintering stage, pass into the H that is less than 15ml/min in protective atmosphere
2.
6. matrix material according to claim 1, is characterized in that: described Mg
2the relative density that Si strengthens the Mg alloy composite materials is at least 98.5%, and tensile strength is at least 470MPa, and unit elongation is at least 12%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103894612A (en) * | 2014-04-01 | 2014-07-02 | 中国石油大学(华东) | Preparation method of soluble Mg2Si-radical high-strength light-weight balls for oil-gas fracturing |
| CN104928510A (en) * | 2015-06-30 | 2015-09-23 | 西安交通大学 | Preparation method of fine-grain Mg-based composite material comprising AlN (aluminum nitride) particles |
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|---|---|---|---|---|
| JP2000017352A (en) * | 1998-06-26 | 2000-01-18 | Toyota Central Res & Dev Lab Inc | Magnesium base composite material |
| JP2004225080A (en) * | 2003-01-21 | 2004-08-12 | Center For Advanced Science & Technology Incubation Ltd | Magnesium silicide-containing magnesium alloy, method of producing the same, and method of forming magnesium silicide |
| CN1556868A (en) * | 2001-09-25 | 2004-12-22 | ��ʽ���綫����ѧTLO | Magnesium base composite material |
| CN1735472A (en) * | 2003-01-08 | 2006-02-15 | 株式会社东京大学Tlo | Magnesium composite powder and manufacture method thereof and magnesium base composite material and manufacture method thereof |
| CN1980760A (en) * | 2004-07-08 | 2007-06-13 | 株式会社东京大学Tlo | Magnesium-base composite powder, magnesium-base alloy material and method for production thereof |
| CN101781720A (en) * | 2009-12-28 | 2010-07-21 | 西安理工大学 | Preparation method of Mg2Si reinforced magnesium alloy |
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2013
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Patent Citations (6)
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|---|---|---|---|---|
| JP2000017352A (en) * | 1998-06-26 | 2000-01-18 | Toyota Central Res & Dev Lab Inc | Magnesium base composite material |
| CN1556868A (en) * | 2001-09-25 | 2004-12-22 | ��ʽ���綫����ѧTLO | Magnesium base composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103894612A (en) * | 2014-04-01 | 2014-07-02 | 中国石油大学(华东) | Preparation method of soluble Mg2Si-radical high-strength light-weight balls for oil-gas fracturing |
| CN104928510A (en) * | 2015-06-30 | 2015-09-23 | 西安交通大学 | Preparation method of fine-grain Mg-based composite material comprising AlN (aluminum nitride) particles |
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