CN104152891A - Method for rapidly forming metallurgical alloy layer on magnesium alloy surface - Google Patents
Method for rapidly forming metallurgical alloy layer on magnesium alloy surface Download PDFInfo
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Abstract
The invention relates to a method for rapidly forming a metallurgical alloy layer on a magnesium alloy surface. In order to overcome the conditions that magnesium alloy is soft in texture and poor in corrosion resistance, a method that a magnesium aluminum alloy layer is sprayed on the surface of an inner cavity of a metal mould in advance is adopted, then, a pressure casting method is utilized for enabling AZ91D magnesium alloy to be formed in the mould, the magnesium aluminum alloy layer which is sprayed in advance is tightly connected with a pressure-casting AZ91D base material through a metallurgical bond and a mechanical lock, and therefore a magnesium aluminum metallurgy alloy layer with the protection effect is formed on the surface of the pressure-casting AZ91D metallurgical alloy layer. According to the method, the surface strength, hardness and corrosion resistance of the magnesium alloy are greatly improved. The corrosion rate of the surface alloy layer is about 12.6 percent of that of the base material, and the abrasion performance can be improved by one time. The manufacturing method is simple in process, the quantity value is complete and accurate, the coating bonding strength is good, the tissue is compact, the pressure-casting magnesium alloy coating enhanced method is quite ideal, and batch production and application in the magnesium alloy pressure-casting industry can be achieved.
Description
Technical field
The present invention relates to a kind of method that Mg alloy surface forms metallurgical alloy layer fast, belong to non-ferrous metal and improve technical field prepared by corrosion resisting property and technique.
Background technology
Magnesium and magnesium alloy are a kind of non-ferrous metal alloys, have density little, and specific tenacity and specific rigidity are high, and electromagnetic wave shielding is good, are easy to the advantages such as processing, at automotive industry, electronic product, aerospace field, are used widely; But its chemically reactive is high, corrosion-resistant, in malaria, very easily oxidation generates loose porous oxide film, and these drawbacks have limited the application of magnesium alloy in more areas, in order to make magnesium alloy obtain application more widely, magnesium alloy is carried out to surface treatment and be very important.
At present, the surface treatment method of magnesium alloy has various ways, as chemical conversion facture, anodic oxidation treatment method, organic coating method, PVD method, plating, surface spraying metal etc., although these surface modifying methods have certain effect to magnesium alloy, but also there is technical deficiency, some complex process, facility investment is large, cost is high, and some coatings and matrix associativity are poor, easily come off, some coated substance performances are not enough, do not reach enhancing, Hardening, corrosion resistant object, in a word, major part is all difficult to realize heavy industrialization application.
Summary of the invention
The present invention, for technical problems such as complex process, coated substance performance deficiencies in the process for treating surface of the current magnesium alloy of solution, provides a kind of Mg alloy surface to form fast the method for metallurgical alloy layer.
The present invention adopts following technical scheme to realize: a kind of Mg alloy surface forms the method for metallurgical alloy layer fast, adopts following raw material: AZ91D magnesium alloy ingot, magnesium powder, aluminium powder, argon gas;
Comprise the following steps:
(1) selected chemical substance material
As follows to the chemical substance quality of materials control of purity using:
AZ91D magnesium alloy ingot: solid-state solid is more than 99.9%;
Magnesium powder: solid-state solid is more than 99.9%;
Aluminium powder: solid-state solid is more than 99.9%;
(2) alloying of coating casting
1. prepare retractable die
With stainless material, prepare retractable die, die cavity is rectangle, and adds filter screen at sprue gate;
2. alloying casting
The magnesium powder and the aluminium powder that take equal in quality, be placed in smelting pot;
Open smelting furnace, be heated to 780 ℃ ± 5 ℃, make magnesium aluminium powder fusing, at this temperature constant temperature insulation 15min ± 1min, become magnalium solution, open argon bottle, aim at smelting pot input argon gas, argon gas input speed 100 ± 5cm
3/ min, when temperature is down to 720 ℃ ± 5 ℃, starts casting;
3. be cast into ingot
The crucible that fills magnalium liquation is aimed to retractable die and cast, till watering completely;
4. cooling
By casting after retractable die be placed in natural air environment carry out cooling, to room temperature;
5. ingot is got in die sinking
Open retractable die, take out ingot casting;
(3) ball grinds
Ingot casting is broken into fragment, be then placed in ball mill and carry out ball milling, ball milling pill-rolling material is GCr15 steel; Ball milling pill-rolling is 10:1 with the ratio of bulk material volume, and rotational speed of ball-mill is 290～310r/min, Ball-milling Time 60min; Then with 1250 eye mesh screens, sieve, the particle by screen cloth does not continue ball milling, after ball milling 60min, after sieve, repeatedly carries out, until powder reaches the amount of use, last magnalium fine particle diameter is less than 10 μ m;
(4) die casting inner chamber spraying
Adopt cold spray-coating method, the magnalium mixing fine powders preparing in the spraying of die casting surface of internal cavity; Use N
2as accelerating gas, the pressure at nozzle place is 2MPa, and temperature is 150 ℃; The distance of nozzle distance die casting internal surface is 18～22mm, and the speed that in spraying process, spray gun moves is 80 ± 4mm/s;
(5) die cast
The AZ91D magnesium alloy of melting is injected to the die casting that internal surface is coated with magnesium aluminum-alloy powder, the temperature of the magnesium alloy of melting is 650 ± 20 ℃, AZ91D magnesium alloy pressure-casting completes on a cold-chamber die casting machine, the clamp force of pressure die-casting machine is 6500kN, the temperature of die casting is 280 ± 10 ℃, just obtains the magnesium-alloy material that surface is formed with metallurgical alloy layer after complete press casting procedure.
The present invention compared with prior art has obvious advance; it is feature soft for magnesium alloy quality, corrosion-resistant; adopt in advance at metal die surface of internal cavity spraying magnalium layer; then utilize pressure casting method; make AZ91D magnesium alloy at in-mold molding; by the AZ91D base material of magnalium layer and the die casting of spraying in advance by metallurgical key and the tight combination of mechanical lock, thereby at die casting AZ91D Mg alloy surface formation one deck, there is the magnalium metallurgical alloy layer of provide protection.The preparation method of magnalium mixing fine powders of the present invention can guarantee that the magnalium fine powder of preparing is beneficial to spraying; The parameter that spraying coating process adopts can guarantee that magnalium (mixing fine powders) can closely combine by metallurgical key and mechanical lock in follow-up press casting procedure; The parameter that extrusion process adopts has guaranteed the effect of die casting.The combination of each related process and parameter has finally increased substantially surface strength, hardness and the erosion resistance of magnesium alloy.And the erosion rate of surface alloying layer is approximately 12.6% of base material, its wear resistance can double.
The present invention be take AZ91D magnesium alloy as matrix, adopting magnalium is surface spraying material, through casting magnesium aluminum alloy, ball grinds, mould surface spraying, pressure die casting, diecast magnesium alloy surface forms alloy rete, thereby increases substantially mechanical property and and the corrosion resistance nature of diecast magnesium alloy.The method has been avoided traditionally as obtaining base material tissue variation that diffusion heat treatments that the alloy coat of said function carries out causes and the deterioration of mechanical property.This preparation method's technique is simple, and value is accurately full and accurate, and anchoring strength of coating is good, and dense structure is the coating Enhancement Method of very good diecast magnesium alloy, can in magnesium alloy pressure-casting industry, realize mass production applications.
Accompanying drawing explanation
Fig. 1 is sample surfaces alloy layer preparation process schematic diagram.
Fig. 2 is with the sectional view of surface metallurgic alloy coat sample.
Fig. 3 is the heterogeneous microstructure figure of alloy cpd layer.
Fig. 4 is the EDS line sweep result figure at solid black lines place in Fig. 2.
Fig. 5 is the XRD diffraction spectrogram of die casting AZ91D magnesium alloy base material and surperficial magnalium compound layer.
Fig. 6 be base material and coating sample be immersed in liberation of hydrogen speed in 5wt.%NaCl solution and
Soak time graph of a relation.
Fig. 7 is the polarization curve of base material and magnalium coating.
Fig. 8 is the wear test rear surface SEM shape appearance figure of AZ91D magnesium alloy base material.
Fig. 9 is the wear test rear surface SEM shape appearance figure of magnalium coating.
Embodiment
1 one kinds of Mg alloy surfaces of embodiment form the method for metallurgical alloy layer fast, adopt following raw material: AZ91D magnesium alloy ingot, magnesium powder, aluminium powder, argon gas;
Comprise the following steps:
(1) selected chemical substance material
As follows to the chemical substance quality of materials control of purity using:
AZ91D magnesium alloy ingot: solid-state solid is more than 99.9%;
Magnesium powder: solid-state solid is more than 99.9%;
Aluminium powder: solid-state solid is more than 99.9%;
(2) alloying of coating casting
1. prepare retractable die
With stainless material, prepare retractable die, die cavity is rectangle, and adds filter screen at sprue gate;
2. alloying casting
The magnesium powder and the aluminium powder that take equal in quality, be placed in smelting pot;
Open smelting furnace, be heated to 775 ℃, make magnesium aluminium powder fusing, at this temperature constant temperature insulation 14min, become magnalium solution, open argon bottle, aim at smelting pot input argon gas, argon gas input speed 95cm
3/ min, when temperature is down to 720 ℃, starts casting;
3. be cast into ingot
The crucible that fills magnalium liquation is aimed to retractable die and cast, till watering completely;
4. cooling
By casting after retractable die be placed in natural air environment carry out cooling, to room temperature;
5. ingot is got in die sinking
Open retractable die, take out ingot casting;
(3) ball grinds
Ingot casting is broken into bulk (as 10 * 10mm), is then placed in ball mill and carries out ball milling, ball milling pill-rolling material is GCr15 steel; Ball milling pill-rolling is 10:1 with the ratio of bulk material, and rotational speed of ball-mill is 290r/min, Ball-milling Time 60min; Then with 1250 eye mesh screens, sieve, the particle by screen cloth does not continue ball milling, after ball milling 60min, after sieve, repeatedly carries out, until powder reaches the amount of use, last magnalium fine particle diameter is less than 10 μ m;
(4) die casting inner chamber spraying
Adopt cold spray-coating method, at the previously prepared good magnalium mixing fine powders of die casting surface of internal cavity spraying; Use N
2as accelerating gas, the pressure at nozzle place is 2MPa, and temperature is 150 ℃; The distance of nozzle distance die casting internal surface is 20mm, and the speed that in spraying process, spray gun moves is 76mm/s;
(5) die cast
The AZ91D magnesium alloy of melting is injected to the die casting that internal surface is coated with magnesium aluminum-alloy powder, the temperature of the AZ91D magnesium alloy of melting is 630 ℃, AZ91D magnesium alloy pressure-casting completes on a cold-chamber die casting machine, the clamp force of pressure die-casting machine is 6500kN, the temperature of die casting is 280 ℃, just obtains the magnesium-alloy material that surface is formed with metallurgical alloy layer after complete press casting procedure.
2 one kinds of Mg alloy surfaces of embodiment form the method for metallurgical alloy layer fast, adopt following raw material: AZ91D magnesium alloy ingot, magnesium powder, aluminium powder, argon gas;
Comprise the following steps:
(1) selected chemical substance material
As follows to the chemical substance quality of materials control of purity using:
AZ91D magnesium alloy ingot: solid-state solid is more than 99.9%;
Magnesium powder: solid-state solid is more than 99.9%;
Aluminium powder: solid-state solid is more than 99.9%;
(2) alloying of coating casting
1. prepare retractable die
With stainless material, prepare retractable die, die cavity is rectangle, and adds filter screen at sprue gate;
2. alloying casting
The magnesium powder and the aluminium powder that take equal in quality, be placed in smelting pot;
Open smelting furnace, be heated to 780 ℃, make magnesium aluminium powder fusing, at this temperature constant temperature insulation 16min, become magnalium solution, open argon bottle, aim at smelting pot input argon gas, argon gas input speed 100cm
3/ min, when temperature is down to 715 ℃, starts casting;
3. be cast into ingot
The crucible that fills magnalium liquation is aimed to retractable die and cast, till watering completely;
4. cooling
By casting after retractable die be placed in natural air environment carry out cooling, to room temperature;
5. ingot is got in die sinking
Open retractable die, take out ingot casting;
(3) ball grinds
Ingot casting is broken into fragment, be then placed in ball mill and carry out ball milling, ball milling pill-rolling material is GCr15 steel; Ball milling pill-rolling is 10:1 with the ratio of bulk material volume, and rotational speed of ball-mill is 300r/min, Ball-milling Time 60min; Then with 1250 eye mesh screens, sieve, the particle by screen cloth does not continue ball milling, after ball milling 60min, after sieve, repeatedly carries out, until powder reaches the amount of use, last magnalium fine particle diameter is less than 10 μ m;
(4) die casting inner chamber spraying
Adopt cold spray-coating method, at the previously prepared good magnalium mixing fine powders of die casting surface of internal cavity spraying; Use N
2as accelerating gas, the pressure at nozzle place is 2MPa, and temperature is 150 ℃; The distance of nozzle distance die casting internal surface is 18mm, and the speed that in spraying process, spray gun moves is 84mm/s;
(5) die cast
The AZ91D magnesium alloy of melting is injected to the die casting that internal surface is coated with magnesium aluminum-alloy powder, the temperature of the AZ91D magnesium alloy of melting is 650 ℃, AZ91D magnesium alloy pressure-casting completes on a cold-chamber die casting machine, the clamp force of pressure die-casting machine is 6500kN, the temperature of die casting is 290 ℃, just obtains the magnesium-alloy material that surface is formed with metallurgical alloy layer after complete press casting procedure.
3 one kinds of Mg alloy surfaces of embodiment form the method for metallurgical alloy layer fast, adopt following raw material: AZ91D magnesium alloy ingot, magnesium powder, aluminium powder, argon gas;
Comprise the following steps:
(1) selected chemical substance material
As follows to the chemical substance quality of materials control of purity using:
AZ91D magnesium alloy ingot: solid-state solid is more than 99.9%;
Magnesium powder: solid-state solid is more than 99.9%;
Aluminium powder: solid-state solid is more than 99.9%;
(2) alloying of coating casting
1. prepare retractable die
With stainless material, prepare retractable die, die cavity is rectangle, and adds filter screen at sprue gate;
2. alloying casting
The magnesium powder and the aluminium powder that take equal in quality, be placed in smelting pot;
Open smelting furnace, be heated to 785 ℃, make magnesium aluminium powder fusing, at this temperature constant temperature insulation 15min, become magnalium solution, open argon bottle, aim at smelting pot input argon gas, argon gas input speed 105cm
3/ min, when temperature is down to 725 ℃, starts casting;
3. be cast into ingot
The crucible that fills magnalium liquation is aimed to retractable die and cast, till watering completely;
4. cooling
By casting after retractable die be placed in natural air environment carry out cooling, to room temperature;
5. ingot is got in die sinking
Open retractable die, take out ingot casting;
(3) ball grinds
Ingot casting is broken into fragment, be then placed in ball mill and carry out ball milling, ball milling pill-rolling material is GCr15 steel; Ball milling pill-rolling is 10:1 with the ratio of bulk material, and rotational speed of ball-mill is 310r/min, Ball-milling Time 60min; Then with 1250 eye mesh screens, sieve, the particle by screen cloth does not continue ball milling, after ball milling 60min, after sieve, repeatedly carries out, until powder reaches the amount of use, last magnalium fine particle diameter is less than 10 μ m;
(4) die casting inner chamber spraying
Adopt cold spray-coating method, at the previously prepared good magnalium mixing fine powders of die casting surface of internal cavity spraying; Use N
2as accelerating gas, the pressure at nozzle place is 2MPa, and temperature is 150 ℃; The distance of nozzle distance die casting internal surface is 22mm, and the speed that in spraying process, spray gun moves is 80mm/s;
(5) die cast
The AZ91D magnesium alloy of melting is injected to the die casting that internal surface is coated with magnesium aluminum-alloy powder, the temperature of the AZ91D magnesium alloy of melting is 670 ℃, AZ91D magnesium alloy pressure-casting completes on a cold-chamber die casting machine, the clamp force of pressure die-casting machine is 6500kN, the temperature of die casting is 270 ℃, just obtains the magnesium-alloy material that surface is formed with metallurgical alloy layer after complete press casting procedure.
Complete press casting procedure comprises: matched moulds, die casting, die sinking, eject and take out sample.
Also comprise the storage to product: the magnalium coating sample to preparation is packed with soft dust-free paper, is placed in moisture-resistant cabinet, with waterproof, protection against the tide, anti-oxidation, anti-acid-alkali salt, corrode, storing temp is 20 ℃ ± 2 ℃, relative temperature≤10%.
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, it is sample surfaces alloy layer preparation process schematic diagram.First by pure magnesium powder and pure aluminium powder fusing, cast magnalium, then with grinding of ball grinder, become particle diameter to be less than the powder of 10 μ m, then at the surface of internal cavity of mould, deposit the good magnalium coating of ball milling, last die cast AZ91D magnesium alloy sample by the method for cold spraying.
Shown in Fig. 2, it is the microtexture sectional view of the alloy cpd layer of diecast magnesium alloy sample surfaces.As seen from the figure: because coating outside surface is release, therefore relatively smooth, and interface between coating and base material is uneven, this is because the feature of spraying self causes.This rough interface exactly, for coating and base material are in conjunction with providing mechanical lock, have increased the bonded area of coating and base material, thereby has improved the bonding strength between coating and base material.In addition, the coating that this method produces has also produced metallurgical key, for the combination between coating and base material provides favourable condition.Therefore, this method is all converted into the unfavorable factor in spraying and die casting the favorable factor of coating combination, the more important thing is, has successfully avoided the impact of high-temperature heat treatment on base material weave construction and mechanical property, and thermal treatment is the approach that obtains metallurgical diffusion layer.
Shown in Fig. 3, be the micro-structure diagram of magnalium compound layer, this is the pattern after corroding by basic solution, has as seen micropore (0.1-0.3 μ m) to exist in coating.These micropore positions may be the positions that aluminium particulate exists.
Shown in Fig. 4, it is the line sweep collection of illustrative plates of magnalium layer.The weight ratio of EDS analytical results explanation Mg and Al is 49.6/50.4, and this shows that in alloy coat, major part is β-Mg
17al
12.
Shown in Fig. 5, be the XRD diffraction spectrogram of die casting AZ91D magnesium alloy base material and surperficial magnalium compound layer, as seen from the figure: the main component of coating is intermetallic compound β-Mg that magnalium forms
17al
12, also having the seldom Al of amount, this is consistent with SEM observations.
Shown in Fig. 6, for base material and coating sample are immersed in liberation of hydrogen speed and the soak time graph of a relation in 5wt.% NaCl solution.Visible, with the prolongation of soak time, AZ91D magnesium alloy base material not only corrodes gradually, but also presents the trend of accelerated corrosion gradually.Yet almost there is not corrosion in coating sample.
Shown in Fig. 7, for having Mg through electrokinetic potential sweep test acquisition die casting AZ91D magnesium alloy substrate and surface
17al
12the polarization curve of coating sample in 3.5wt.%NaCl solution, can obviously find out that from figure protection due to coating makes the corrosion potential of the sample 340mV that shuffles, and corrosion electric current density 1 order of magnitude that all declines, and belongs to typical anodic control protection.According to Ta Feier epitaxial method, can calculate, the erosion rate of coating sample is only 12.6% of substrate sample.
Shown in Fig. 8, it is SEM surface topography after the wear-resistant experiment of base material.Visible: in AZ91D base material, polishing scratch rule, that ditch dug with a plow is the same of mainly take is feature, there is no the vestige of plasticity hangover shape, is the feature that belongs to abrasive wear in a word.The width of polishing scratch is 821 μ m.Shown in Fig. 9, be SEM surface topography map after the wear-resistant experiment of magnalium coating, obviously visible, coating sample presents the feature of an obvious adhesion wear.The width of polishing scratch is 462 μ m.Find with the SEM pattern contrast of base material, the wear resisting property of coating is greatly improved.
Claims (2)
1. Mg alloy surface forms a method for metallurgical alloy layer fast, it is characterized in that: adopt following raw material: AZ91D magnesium alloy ingot, magnesium powder, aluminium powder, argon gas;
Comprise the following steps:
(1) selected chemical substance material
As follows to the chemical substance quality of materials control of purity using:
AZ91D magnesium alloy ingot: solid-state solid is more than 99.9%;
Magnesium powder: solid-state solid is more than 99.9%;
Aluminium powder: solid-state solid is more than 99.9%;
(2) alloying of coating casting
1. prepare retractable die
With stainless material, prepare retractable die, die cavity is rectangle, and adds filter screen at sprue gate;
2. alloying casting
The magnesium powder and the aluminium powder that take equal in quality, be placed in smelting pot;
Open smelting furnace, be heated to 780 ℃ ± 5 ℃, make magnesium aluminium powder fusing, at this temperature constant temperature insulation 15min ± 1min, become magnalium solution, open argon bottle, aim at smelting pot input argon gas, argon gas input speed 100 ± 5cm
3/ min, when temperature is down to 720 ℃ ± 5 ℃, starts casting;
3. be cast into ingot
The crucible that fills magnalium liquation is aimed to retractable die and cast, till watering completely;
4. cooling
By casting after retractable die be placed in natural air environment carry out cooling, to room temperature;
5. ingot is got in die sinking
Open retractable die, take out ingot casting;
(3) ball grinds
Ingot casting is broken into fragment, be then placed in ball mill and carry out ball milling, ball milling pill-rolling material is GCr15 steel; Ball milling pill-rolling is 10:1 with the ratio of bulk material volume, and rotational speed of ball-mill is 290～310r/min, Ball-milling Time 60min; Then with 1250 eye mesh screens, sieve, the particle by screen cloth does not continue ball milling, after ball milling 60min, after sieve, repeatedly carries out, until powder reaches the amount of use, last magnalium fine particle diameter is less than 10 μ m;
(4) die casting inner chamber spraying
Adopt cold spray-coating method, the magnalium mixing fine powders preparing in the spraying of die casting surface of internal cavity; Use N
2as accelerating gas, the pressure at nozzle place is 2MPa, and temperature is 150 ℃; The distance of nozzle distance die casting internal surface is 18～22mm, and the speed that in spraying process, spray gun moves is 80 ± 4mm/s;
(5) die cast
The AZ91D magnesium alloy of melting is injected to the die casting that internal surface is coated with magnesium aluminum-alloy powder, the temperature of the magnesium alloy of melting is 650 ± 20 ℃, AZ91D magnesium alloy pressure-casting completes on a cold-chamber die casting machine, the clamp force of pressure die-casting machine is 6500kN, the temperature of die casting is 280 ± 10 ℃, just obtains the magnesium-alloy material that surface is formed with metallurgical alloy layer after complete press casting procedure.
2. a kind of Mg alloy surface as claimed in claim 1 forms the method for metallurgical alloy layer fast, it is characterized in that, complete press casting procedure comprises: matched moulds, die casting, die sinking, eject and take out sample.
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| CN112570687A (en) * | 2019-09-29 | 2021-03-30 | 洛阳钢丰机械制造有限公司 | Special alloy composite casting process |
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| CN113199010A (en) * | 2021-04-26 | 2021-08-03 | 中国兵器工业第五九研究所 | Method for alloying magnesium element on surface layer of aluminum alloy casting |
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