CN105238943B - In-situ reinforcement preparation method and device for high-strength and high-ductility casting magnesium-based composite material - Google Patents
In-situ reinforcement preparation method and device for high-strength and high-ductility casting magnesium-based composite material Download PDFInfo
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- CN105238943B CN105238943B CN201510670943.XA CN201510670943A CN105238943B CN 105238943 B CN105238943 B CN 105238943B CN 201510670943 A CN201510670943 A CN 201510670943A CN 105238943 B CN105238943 B CN 105238943B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 239000011777 magnesium Substances 0.000 title claims abstract description 30
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 27
- 238000005266 casting Methods 0.000 title claims abstract description 9
- 238000011065 in-situ storage Methods 0.000 title abstract description 12
- 230000002787 reinforcement Effects 0.000 title abstract description 3
- 239000000956 alloy Substances 0.000 claims abstract description 46
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 45
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 29
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000003723 Smelting Methods 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 238000005728 strengthening Methods 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007499 fusion processing Methods 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 238000013022 venting Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 19
- 239000002245 particle Substances 0.000 abstract description 8
- 229910003023 Mg-Al Inorganic materials 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 4
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 19
- 239000000470 constituent Substances 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000005275 alloying Methods 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 5
- 230000003014 reinforcing effect Effects 0.000 description 5
- 238000009423 ventilation Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 229910021323 Mg17Al12 Inorganic materials 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- -1 is mingled with Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 210000003437 trachea Anatomy 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The invention relates to an in-situ reinforcement preparation method and device for a high-strength and high-ductility casting magnesium-based composite material. Mg-9%Al alloy is adopted as matrix alloy, nitrogen is introduced in an alloy melt in a vacuum smelting resistance furnace, so that the nitrogen and the alloy melt are in gas/gas and gas/liquid reaction, AlN particles evenly distributed are formed in the alloy melt in situ, and therefore the AlN/Mg composite material with the highest extension strength of 193 Mpa and elongation with 14% is prepared. The process and preparation device have the characteristics of being easy to operate, environmentally friendly, low in cost, small in energy consumption and short in preparation period. The strength and ductility of the prepared magnesium-based composite material are superior to those of corresponding Mg-Al alloy (AZ91D), and density is smaller.
Description
Technical field
The present invention relates to a kind of technology of preparing of casting magnesium base composite material, more particularly to using in-situ preparation reinforcing
Grain obtains the magnesium alloy materials of excellent performance improving Properties of Magnesium Alloy.
Background technology
The present invention is to improve or improve conjunction using the principle that equally distributed hardening constituent is generated in alloy melt situ
The performance of gold, mainly for the preparation of aluminium base and magnesium base composite material.Home position strengthening technology in the present invention is applied in aluminium alloy
Comparative maturity, had part commercial production.The shortcomings of having inflammable and oxidizable yet with magnesium alloy, in-situ preparation is strong
Change phase technology and only reside within laboratory stage, and due to the hardening constituent unstable properties for being formed, skewness is sharp at present
The magnesium base composite material tensile property prepared with the technology is not reported accordingly in international and domestic various documents, is only
Tissue description and the test of hardness performance are carried out to it, and performance is less than matrix alloy, thus production is not used at all.
Although and the present invention using with domestic and international correlation technique identical principle, the present invention originally devises alloy
Preparation facilitiess, and by being mutually formed in situ the systematic study of mechanism to particle strengthening, it was found that except gas traditionally-
Two reactions of gas and solid-liquid are formed outside the mechanism of hardening constituent AlN, also there is solution-air and solid-liquid reaction mechanism, and after send out
Existing mechanism is the major way to form hardening constituent AlN, and this allows for AlN and is more prone in the melt to be formed and be uniformly distributed.
In addition, the present invention is it has also been found that by forming hardening constituent AlN, can suppress Mg-Al eutectic reactions, thus eutectic can be greatly decreased
Product Mg17Al12, it is hard crisp phase, is the unfavorable factor for affecting Mg-Al alloy properties to improve.And, by hardening constituent AlN
Formation, the crystallite dimension of matrix alloy obtained effective reduction, and this is also another breakthrough of the present invention.
On this basis, the present invention solves fusant reaction by updating and perfect to preparation facilitiess and technique
It is insufficient, the problems such as be difficult to precise control and many casting defect.Just because of the present invention in hardening constituent Forming Mechanism and preparation
The creative discovery and invention of device and process aspect so that the mechanical property of alloy is greatly improved, its as cast condition is drawn
The AZ91D alloys of intensity and plasticity far super close alloying component are stretched, and due to not adding other alloying elements, its is close
Degree is again smaller than AZ91D alloys.Further, since process is simple, preparation facilitiess are safe and reliable, without pollution, processing ease the features such as,
The invention can be rapidly used for commercial production.
The content of the invention
The technical problem to be solved
In order to avoid the problem that magnesium alloy and performance of magnesium-based composite material are low, particularly situ Particles reinforcing magnesio
Composite, is mingled with, particle strengthening distributed mutually is uneven, course of reaction is difficult to control due to there is oxide in its preparation process
System, cast defect is more, seriously polluted, and the problems such as preparation cost is high, the present invention proposes that a kind of High-strength high-plasticity casts magnesio
The home position strengthening preparation method of composite and device.
Technical scheme
A kind of High-strength high-plasticity casts the home position strengthening preparation method of magnesium base composite material, it is characterised in that step is as follows：
Step 1：By matrix alloy vacuum be 2.0 × 10-2Add hot smelting under MPa, argon work is passed through in fusion process
Protection；Melting to 730 DEG C～780 DEG C are passed through nitrogen toward melt 2～4 hours, every 40 to 60 minutes to molten in venting process
Body carries out 3～5 minutes stirring, and described matrix alloy is Mg-9Al alloys, and quality is 0.8～1.5kg；
Step 2：Melt is cooled in atmosphere room temperature and obtains alloy cast ingot, argon is passed through in cooling procedure and is protected；
Step 3：By the melting again at 700 DEG C～750 DEG C of the alloy cast ingot after cooling, argon work is passed through in fusion process
Protection；Then at 720 DEG C～740 DEG C, casting obtains magnesium base composite material.
A kind of High-strength high-plasticity casts the home position strengthening preparation facilitiess of magnesium base composite material, including thermocouple, pressure gauge, puts
Air valve, vacuum-pumping tube, reative cell, crucible, Ar gas breather and N2Breather；Crucible is located at the bottom of reative cell, thermocouple, takes out
Vacuum tube, Ar gas breather and N2Breather is passed into reaction interior, and vacuum-pumping tube is provided with pressure gauge and vent valve；Its feature
It is also to include moist closet, multichannel passage and stirring vane；Separate a space on reative cell as moist closet, N2It is logical
Trachea is provided with stirring vane, multichannel passage and N on the indoor part of reaction2The bottom of breather is connected.
Beneficial effect
A kind of home position strengthening preparation method and device of High-strength high-plasticity casting magnesium base composite material proposed by the present invention, institute
The magnesium base composite material of preparation, mainly by two phase compositions, i.e. hardening constituent AlN and magnesium matrix.Because the formation of hardening constituent AlN suppresses
The formation of eutectic product Mg17Al12 phases, and this mutually belongs to hard crisp phase, its exist will infringement material performance.Further, since
Hardening constituent AlN has similar crystal structure to magnesium, thus can be brilliant so as to refine magnesium matrix as the heterogeneous equiax crystal of magnesium
Grain.The presence of these Solidification Characteristics allows in-situ preparation to obtain the performance that AlN effectively improves matrix alloy.In cast alloy
On energy, compare with AZ91D alloys (its alloying component is close with alloying component of the present invention, that is, be Mg-9at.%Al), the present invention
The tensile property of the composite of preparation is 180-193MPa, and its percentage elongation is 13-15%, the remote super AZ91D's of difference
160MPa and 2%, and alloy prepared by the present invention, not through refine and heat treatment, its density is again smaller than AZ91D alloys.This
It is also performance highest in had been reported that magnesium base composite material, therefore, the realization of the present invention will greatly expand making for magnesium alloy
With scope, the low problem of energy effectively solving Properties of Magnesium Alloy.
In addition, the technology of preparing of the present invention, because whole melting preparation process is carried out in vacuum tightness environment, green
Environmental protection, without pollution, the reaction gas for using is nitrogen, and low cost is safe from danger.Reaction temperature be 700-800 degree between, with
Conventional magnesium alloy smelting temperature is consistent, does not increase energy consumption, and compares conventional fabrication process, and the technology of the present invention is eliminated to be removed
The links such as slag, refine, thus preparation efficiency is higher.
Description of the drawings
The preparation facilitiess of Fig. 1 original positions magnesium base composite material
1- thermocouples；2- pressure gauges；3- vent valves；4- evacuation；5- vacuum chambers and reative cell；6- crucibles；7- passages；
8- stirring vanes；9-Ar gas entrances；10- moist closets；11-N2Breather
Fig. 2 is tensile sample piece
Fig. 3 is tensile sample chip size figure
Fig. 4 is as-cast structure stress-strain curve diagram
Fig. 5 is the macrograph of situ Al N/Mg composite
Fig. 6 is the XRD analysis collection of illustrative plates of situ Al N/Mg composite
Specific embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described：
The technical scheme is that and set up on the ultimate principle for generating reinforcing particle in magnesium alloy fused mass situ, but
If simply reacting gas nitrogen is passed through in magnesium alloy fused mass, hardening constituent AlN can not be formed in magnesium alloy fused mass, and
It is only capable of forming a thin layer AlN in bath surface, due to the passivation of AlN, alloy melt inside AlN is difficult to be formed, and this is also
The core that the international and domestic technology cannot obtain continuing to develop is located.The present invention is directed to this principle, originally devises system
Standby device：Install moist closet additional on vacuum chamber top first, efficiently solve gas tube and thermocouple in melting and course of reaction
In move up and down the problem for easily causing gas leakage and air inlet；Second, install vent valve and relief valve additional on moist closet, when
Gas pressure in vacuum room can reduce room pressure beyond certain limit by deflating, so as to ensure whole preparation process
Safety.3rd, Multiple-Aperture Device is designed and is mounted with breather lower end, by certain aperture, can obtain in alloy melt
Tiny and equally distributed bubble is obtained, is conducive to bubble to the stirring of melt and is accelerated the response speed of bubble and melt.
4th, install blade additional in breather lower end, can be realized to melt by rotation breather during gas-liquid reaction
Mechanical agitation, accelerates reaction and reinforcing particle to be uniformly distributed.
In addition, through testing repeatedly and analysis result, it is determined that optimal technological parameter, such as temperature range, duration of ventilation
And ventilation etc., it can be ensured that whole preparation method normally complete and composite property raising.
Fig. 1 is the preparation facilitiess schematic diagram of homemade magnesium base composite material in situ, it can be seen that magnesium alloy melts in crucible
Refining, and react with nitrogen, form AlN hardening constituents.By Gas Stirring and mechanical agitation, the AlN hardening constituents of formation can be with
In being evenly distributed on alloy melt.
As described in Figure 1, the device is generally made up of upper and lower two parts, above be moist closet 10, below for vacuum chamber with
Reative cell 5；Thermometric in metal bath in the insertion crucible 6 of thermocouple 1 on top；N2Breather 11 and stirring vane 8, ventilation
Hole 7 constitutes breather and agitating device, can ventilate and stir, and accelerates in melt the synthesis speed of particle strengthening phase and uniform
Distribution；Following vacuum chamber and reative cell 5 is integrated, can be with dual-purpose；Pressure gauge 2 above right-hand member can be with the pressure in display device
Power；Evacuation 4 connects evacuator, to device evacuation；Vent valve 3 can deflate, it is ensured that the pressure in device, it is ensured that experiment peace
Entirely, safety device is belonged to；Ar gas 9 leads to Ar gas, protects alloy melt.
The device collection vacuum chamber 5, moist closet 10, reative cell 5, agitating device 7,8,11, safety guard 3, ventilation are filled
7,8,11 are put in one；Moist closet 10 is in reative cell and the top of vacuum chamber 5, it is ensured that anti-in magnesium base composite material preparation process in situ
Answer melt temperature in room 5 uniform, manufacturing cycle, while can be beneficial to reduce the heating-up time, can be shortened with precise control reaction temperature,
So as to improve preparation efficiency.The bottom of breather 11 is a Multi-hole air filling device 7, single channel gas can be converted to multichannel gas
Body, reduces the size of reaction bubble, increases number of bubbles, stirs with the reaction of melt and to melt so as to be beneficial to bubble
Mix, be conducive to the quick formation of hardening constituent.Breather lower end adds stirring vane 8, it is possible to move in a circle (rotation) with
And lengthwise movement so that stir and ventilate in one, while can effectively realizing that melt forms hardening constituent with gas reaction, promote
Reinforcing particle is evenly distributed in melt.Equipped with vacuometer 2, air gauge 2, relief valve 3, thermocouple 1 outside device, effectively protect
Accuracy and the safety of fusant reaction control are demonstrate,proved.
The device has following feature：
A the () equipment integrates vacuum chamber, moist closet, reative cell, agitating device, safety guard, breather；
B () agitating device can need to realize the stirring of melt longitudinal direction and circumferencial direction according to technique；
C () breather bottom is Multiple-Aperture Device, be capable of achieving to be changed into multi-channel gas this conversions from the gas of single channel,
The contact area of melt and bubble is increased, while also acting as the effect that bubble is sufficiently stirred for melt；
D () alloy melting and reaction in-situ are carried out under vacuum chamber and argon protection, reacting gas is nitrogen, therefore,
It is whole preparation process alloy melt non-oxidation, pollution-free, and safety and environmental protection.
Specific implementation process of the present invention is as follows：
1st, using alloy based on Mg-9Al alloys, shielding gas is argon, and nitrogen is reacting gas.
2nd, the preparation of composite is carried out using homemade magnesium base composite material Preparation equipment in situ in resistance furnace：Will
The matrix alloy of 0.8～1.5kg is put in crucible, then crucible is placed in vacuum chamber as shown in Figure 1, then will be such as Fig. 1 institutes
The preparation facilitiess for showing are put in resistance furnace, close inflatable and deflatable valve, with mechanical pump by vacuum chamber to 2.0x10-2MPa。
3rd, opening resistor stove is heated to vacuum chamber, when melt temperature is 730 DEG C～780 DEG C, closes vacuum valve, is stopped
Only evacuation, then inserts nitrogen breather in alloy melt, and a certain amount of nitrogen is continually fed in alloy melt.
4th, during logical nitrogen, periodically move up and down at a slow speed and rotate breather and (moved down on 40 to 60 minutes
Dynamic and rotating stirring device 3～5 minutes), periodic low rate mixing is carried out to alloy melt.
5th, lead to after the nitrogen time reaches 2～4 hours, breather is carried to melt top, and stop inflation.
6th, after ventilation terminates, preparation facilitiess are taken out from resistance furnace, under the protection of argon, room is cooled in atmosphere
Temperature.
7., by the remelting at 700 DEG C～750 DEG C of the alloy cast ingot after cooling, argon is passed through in fusion process and is protected；So
Cast at 720 DEG C～740 DEG C afterwards.
It can be seen that by using the preparation facilitiess of the present invention, concrete technology is simple, easily operated, safety and environmental protection, without discarded
With the generation of waste residue.Magnesium base composite material stable mechanical property prepared by the present invention, and also have the space further improved.
By the preparation facilitiess of homemade magnesium base composite material in situ, with the preparation technology of the present invention, we obtain
The casting AlN/Mg-Al composites of excellent performance, the composite possesses high intensity and high plasticity, can be used directly to
Use as cast magnesium alloy, it is also possible to do wrought magnesium alloy and use.Because our matrix alloy is Mg-9Al alloys, it is close to
AZ91 alloying components in cast magnesium alloy system, table 1 gives high-strength high-plasticity magnesium alloy obtained in this patent and AZ91
The contrast of magnesium alloy mechanical property.
The AlN/Mg composites of table 1 are contrasted with GB AZ91D As-cast Microstructure mechanical property
The present invention adopts vacuum melting, and argon protection, reacting gas are nitrogen, matrix alloy adopts Mg-Al bianry alloys,
Whole melting and material are prepared and carried out in hermetic container, thus, there is no magnesium alloy burning and need the feelings of SF6 gas shields
Condition, magnesium alloy fused mass is not in the problem that oxide is mingled with, and be passed through melt gas be drying nitrogen, low cost.This
The preparation technology parameter of invention is only melt temperature and gas flow, because technological parameter is easily controlled, thus present invention solution
In-sltu reinforcement magnesium base composite material of having determined research only resides within the bottleneck of laboratory stage, can promote the industrialization of magnesium alloy
Production.
Claims (1)
1. a kind of High-strength high-plasticity casts the home position strengthening preparation facilitiess of magnesium base composite material, including thermocouple (1), pressure gauge
(2), vent valve (3), vacuum-pumping tube (4), reative cell (5), crucible (6), Ar gas breathers (9) and N2Breather (11)；Crucible
(6) positioned at the bottom of reative cell (5), thermocouple (1), vacuum-pumping tube (4), Ar gas breathers (9) and N2Breather (11) is passed through
To in reative cell (5), vacuum-pumping tube (4) is provided with pressure gauge (2) and vent valve (3)；Characterized by further comprising moist closet
(10), multichannel passage (7) and stirring vane (8)；Separate a space on reative cell (5) as moist closet (10), N2
Breather (11) is provided with stirring vane (8), multichannel passage (7) and N on the part in reative cell (5)2Breather (11)
Bottom be connected；Preparation process is as follows：
Step 1：By matrix alloy vacuum be 2.0 × 10-2Add hot smelting under MPa, argon is passed through in fusion process and is protected；
Melting to 730 DEG C～780 DEG C are passed through nitrogen toward melt 2～4 hours, in venting process melt are carried out every 40 to 60 minutes
Stir within 3～5 minutes, described matrix alloy is Mg-9Al alloys, quality is 0.8～1.5kg；
Step 2：Melt is cooled in atmosphere room temperature and obtains alloy cast ingot, argon is passed through in cooling procedure and is protected；
Step 3：By the melting again at 700 DEG C～750 DEG C of the alloy cast ingot after cooling, argon is passed through in fusion process and is gone bail for
Shield；Then at 720 DEG C～740 DEG C, casting obtains magnesium base composite material.
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|---|---|---|---|
| CN201510670943.XA CN105238943B (en) | 2015-10-13 | 2015-10-13 | In-situ reinforcement preparation method and device for high-strength and high-ductility casting magnesium-based composite material |
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| CN110373559A (en) * | 2019-08-26 | 2019-10-25 | 上海交通大学 | A kind of method of suitable magnesium and magnesium alloy smelting and casting |
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