CN109266893A - A kind of method of coating zinc oxide graphene enhancing composite material of magnesium alloy - Google Patents

A kind of method of coating zinc oxide graphene enhancing composite material of magnesium alloy Download PDF

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CN109266893A
CN109266893A CN201811104028.4A CN201811104028A CN109266893A CN 109266893 A CN109266893 A CN 109266893A CN 201811104028 A CN201811104028 A CN 201811104028A CN 109266893 A CN109266893 A CN 109266893A
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zinc oxide
coating zinc
oxide graphene
magnesium alloy
graphene
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CN109266893B (en
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袁秋红
廖琳
周国华
林泉博
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JIANGXI TIANYUE AUTOMOBILE ELECTRICAL APPARATUS Co.,Ltd.
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Yichun University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/06Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium

Abstract

A kind of method of coating zinc oxide graphene enhancing composite material of magnesium alloy, the following steps are included: the prefabricated block green body for using liquid dispersed method to prepare the mass ratio of coating zinc oxide graphene and pure aluminium powder first as 10-25%, it is then added in magnesium alloy solution, again after power is the ultrasonic wave decentralized processing 1-20min of 500-1000W, under the conditions of 550-630 DEG C, casting method is used to be prepared for the AZ91 composite material of magnesium alloy that content enhances for 0.1-5% coating zinc oxide graphene.It is uniformly dispersed in magnesium matrix that the present invention can be effectively improved graphene; improve graphene and magnesium matrix interface quality; preferable grain refining effect is obtained simultaneously, and composite materials property promotion amplitude is larger, the graphene-composite material of magnesium alloy haveing excellent performance suitable for prepare with scale.

Description

A kind of method of coating zinc oxide graphene enhancing composite material of magnesium alloy
Technical field
The invention belongs to metallic composite preparation fields, the in particular to preparation method of composite material of magnesium alloy.
Background technique
Composite material of magnesium alloy has specific strength, specific stiffness high, a series of advantages such as damping and wear-resisting property are good, make its The fields such as electronics, aerospace and automobile have huge potential application foreground.It is multiple how high-strength light toughness magnesium alloy is developed Condensation material, it has also become one of research hotspot in Material Field.As the obvious member of nano-sized carbon family, graphene is because of its conduction It is considered as the excellent reinforcement of magnesium alloy with the characteristics such as good heat conductivity, excellent in mechanical performance.Currently, graphene enhances magnesium The research of alloy composite materials is also in the budding stage.As carbon nanotube, the interface of graphene and many metallic matrixes is tied Close weaker and easy reunion.Therefore, graphene-composite material of magnesium alloy that processability is more excellent, first has to solve two The interface bond strength and realization graphene of critical issue, i.e. raising graphene and magnesium are evenly dispersed in magnesium matrix.High temperature Under the conditions of, zinc oxide is easy that interfacial reaction occurs with magnesium, and generating magnesia and two kinds of zinc of interfacial product, magnesia can effectively mention The interface quality of high graphene and magnesium, zinc then form magnesium-zinc intermediate compound with magnesium, improve interface bond strength.In addition, Interfacial reaction further promotes that graphene is evenly dispersed in magnesium solution, while refining the grain structure of magnesium, into And improve the mechanical property of composite material.
Summary of the invention
The object of the present invention is to provide a kind of methods of coating zinc oxide graphene enhancing composite material of magnesium alloy.
The present invention is achieved by the following technical solutions.
A kind of method of coating zinc oxide graphene enhancing composite material of magnesium alloy of the present invention, including following step Suddenly.
(1) coating zinc oxide graphene is pre-dispersed: pressing 1-5g/L concentration ratio, coating zinc oxide graphene is added to second In alcohol or distilled water, ultrasonic 0.5-2h obtains finely dispersed Dispersion of Reinforcement liquid.
(2) ratio for being 10-25: 90-75 in coating zinc oxide graphene and the mass ratio of pure aluminium powder, granularity is less than The pure aluminium powder of 400 mesh is added in dispersion liquid obtained by step (1), obtains coating zinc oxide stone after ultrasound and mechanical stirring 0.5-2h The uniformly mixed slurries of black alkene-aluminium powder.
(3) after to the filtering of slurries obtained by step (2), then the vacuum dried coating zinc oxide graphene-aluminium powder that obtains divides in advance Dissipate uniform mixed-powder.
(4) by mixed-powder obtained by step (3), it is pre-dispersed that coating zinc oxide graphene is made using 300-600MPa pressure More uniform block green compact, be then preheated to 60-100 DEG C it is spare.
(5) prepared by composite material of magnesium alloy: accounting for composite material gross mass by coating zinc oxide graphene addition quality is The magnesium alloy material of 0.1-5%, adds it in crucible, opens power supply and is heated, while uniformly sprinkling in alloy material One layer of RJ2 melting coverture, additional amount are the 0.5-1.5% of magnesium alloy weight.Continue to heat, is warming up to 650-750 to temperature DEG C, after furnace charge is completely melt, 5-15 min is stood, removes surface slag, is uniformly sprinkled in bath surface and is accounted for weight alloy and be The RJ2 coverture of 0.05-0.1% obtains magnesium alloy melt.
(6) temperature of magnesium alloy melt obtained by step (5) is adjusted to after 550-650 DEG C, it is preheated that step (4) is added Coating zinc oxide graphene-aluminium block body green compact, after fusing, temperature rises to 700-800 DEG C of melting 5-30min, and to obtain composite material molten Body.
(7) after Composite Melt temperature obtained by step (6) being down to 550-650 DEG C, under argon gas protection, use power for The ultrasonic wave of 500-1000W, ultrasonic disperse handle 1-20min, obtain the uniform composite material of coating zinc oxide graphene dispersion Melt.
(8) Composite Melt temperature obtained by step (7) is adjusted to 550-630 DEG C, surface slag is removed, in bath surface The RJ2 coverture for accounting for that weight alloy is 0.05-0.1% is uniformly sprinkled, after standing 1-10min, pouring into temperature is 100-200 DEG C In steel die, the magnesium-based composite material of coating zinc oxide graphene enhancing is obtained.
It is uniformly dispersed in magnesium matrix that present invention process can be effectively improved graphene, improves graphene and magnesium matrix circle Face bond quality, while preferable grain refining effect is obtained, composite materials property promotion amplitude is larger, is suitable for scale Excellent graphene-the composite material of magnesium alloy of processability.
Detailed description of the invention
Fig. 1 is the SEM pattern of coating zinc oxide graphene used in the present invention.
Fig. 2 is AZ91 alloy microscopic structure prepared by the present invention.
Fig. 3 is that the content prepared under the conditions of the embodiment of the present invention 1 is that 0.1wt.% coating zinc oxide graphene enhances AZ91 magnesium-based composite material microscopic structure.
Specific embodiment
The present invention will be described further in conjunction with attached drawing by following embodiment.
Embodiment 1.
The method of the coating zinc oxide graphene enhancing composite material of magnesium alloy, as follows.
(1) coating zinc oxide graphene is pre-dispersed: pressing 1g/L concentration ratio, coating zinc oxide graphene is added to ethyl alcohol Or in distilled water, ultrasonic 0.5h obtains finely dispersed Dispersion of Reinforcement liquid.
(2) ratio for being 10: 90 in coating zinc oxide graphene and the mass ratio of pure aluminium powder, by granularity less than 400 purposes Pure aluminium powder is added in dispersion liquid obtained by step (1), obtains coating zinc oxide graphene-aluminium powder after ultrasound and mechanical stirring 0.5h Uniformly mixed slurries.
(3) after to the filtering of slurries obtained by step (2), then the vacuum dried coating zinc oxide graphene-aluminium powder that obtains divides in advance Dissipate uniform mixed-powder.
(4) by mixed-powder obtained by step (3), it is pre-dispersed relatively that coating zinc oxide graphene is made using 300MPa pressure Even block green compact, be then preheated to 60 DEG C it is spare.
(5) prepared by composite material of magnesium alloy: accounting for composite material gross mass by coating zinc oxide graphene addition quality is 0.1% proportional arrangement magnesium alloy material, its magnesium alloy is added in crucible, is opened power supply and is heated, while in alloy material table Face equably sprinkles one layer of RJ2 melting coverture, and additional amount is the 1.0% of weight alloy.Continue to heat, is warming up to 680 to temperature DEG C, after furnace charge is completely melt, stand 10min, remove surface slag, bath surface uniformly sprinkle account for weight alloy be 0.05% RJ2 coverture, obtain cleaner alloy molten solution.
(6) temperature of melt obtained by step (5) is adjusted to after 550 DEG C, step (4) preheated coating zinc oxide is added Graphene-aluminium block body green compact, after fusing, temperature rises to 700 DEG C of melting 5min and obtains Composite Melt.
(7) after Composite Melt temperature obtained by step (6) being down to 550 DEG C, under argon gas protection, importing power is 500W Ultrasonic wave, ultrasonic disperse handle 3min, obtain the uniform Composite Melt of coating zinc oxide graphene dispersion.
(8) Composite Melt temperature obtained by step (7) is adjusted to 550 DEG C, removes surface slag, sprinkles a small amount of covering Agent after standing 3min, pours into the steel die that temperature is 100 DEG C, obtains content as the increasing of 0.1wt.% coating zinc oxide graphene Strong AZ91 magnesium-based composite material.
Mechanics Performance Testing, Vickers hardness 75-95HV are carried out to the composite material, yield strength reaches 170- 220MPa, elongation percentage reach 8.5-11.7%, are a kind of preferable composite materials of mechanical property.
Embodiment 2.
The method of the coating zinc oxide graphene enhancing composite material of magnesium alloy, as follows.
(1) coating zinc oxide graphene is pre-dispersed: pressing 2g/L concentration ratio, coating zinc oxide graphene is added to ethyl alcohol Or in distilled water, ultrasonic 1h obtains finely dispersed Dispersion of Reinforcement liquid.
(2) ratio for being 15: 85 in coating zinc oxide graphene and the mass ratio of pure aluminium powder, by granularity less than 400 purposes Pure aluminium powder is added in dispersion liquid obtained by step (1), and it is mixed that coating zinc oxide graphene-aluminium powder is obtained after ultrasonic and mechanical stirring 1h Close uniform slurries.
(3) after to the filtering of slurries obtained by step (2), then the vacuum dried coating zinc oxide graphene-aluminium powder that obtains divides in advance Dissipate uniform mixed-powder.
(4) by mixed-powder obtained by step (3), it is pre-dispersed relatively that coating zinc oxide graphene is made using 300MPa pressure Even block green compact, be then preheated to 60 DEG C it is spare.
(5) prepared by composite material of magnesium alloy: accounting for composite material gross mass by coating zinc oxide graphene addition quality is 1.0% proportional arrangement magnesium alloy material, adds it in crucible, opens power supply and is heated, while is uniform on alloy material surface Ground sprinkles one layer of RJ2 melting coverture, and additional amount is the 1.0% of weight alloy.Continue to heat, is warming up to 650 DEG C to temperature, furnace After material is completely melt, 10min is stood, removes surface slag, is uniformly sprinkled in bath surface and accounts for the RJ2 that weight alloy is 0.05% Coverture obtains cleaner alloy molten solution.
(6) temperature of melt obtained by step (5) is adjusted to after 600 DEG C, step (4) preheated coating zinc oxide is added Graphene-aluminium block body green compact, after fusing, temperature rises to 750 DEG C of melting 5min and obtains Composite Melt.
(7) after Composite Melt temperature obtained by step (6) being down to 600 DEG C, under argon gas protection, importing power is The ultrasonic wave of 1000W, ultrasonic disperse handle 5min, obtain the uniform Composite Melt of coating zinc oxide graphene dispersion.
(8) Composite Melt temperature obtained by step (7) is adjusted to 580 DEG C, removes surface slag, sprinkles a small amount of covering Agent after standing 3min, pours into the steel die that temperature is 100 DEG C, obtains content as the increasing of 1.0wt.% coating zinc oxide graphene Strong AZ91 magnesium-based composite material.
Mechanics Performance Testing, Vickers hardness 92-125HV are carried out to the composite material, yield strength reaches 210- 248MPa, elongation percentage reach 9-14%, are a kind of composite materials of excellent in mechanical performance.
Embodiment 3
The method of the coating zinc oxide graphene enhancing composite material of magnesium alloy, as follows.
(1) coating zinc oxide graphene is pre-dispersed: pressing 5g/L concentration ratio, coating zinc oxide graphene is added to ethyl alcohol Or in distilled water, ultrasonic 2h obtains finely dispersed Dispersion of Reinforcement liquid.
(2) ratio for being 25: 75 in coating zinc oxide graphene and the mass ratio of pure aluminium powder, by granularity less than 400 purposes Pure aluminium powder is added in dispersion liquid obtained by step (1), and it is mixed that coating zinc oxide graphene-aluminium powder is obtained after ultrasonic and mechanical stirring 2h Close uniform slurries.
(3) after to the filtering of slurries obtained by step (2), then the vacuum dried coating zinc oxide graphene-aluminium powder that obtains divides in advance Dissipate uniform mixed-powder.
(4) by mixed-powder obtained by step (3), it is pre-dispersed relatively that coating zinc oxide graphene is made using 600MPa pressure Even block green compact, be then preheated to 100 DEG C it is spare.
(5) prepared by composite material of magnesium alloy: accounting for composite material gross mass by coating zinc oxide graphene addition quality is 3% Proportional arrangement magnesium alloy material, add it in crucible, open power supply and heated, while uniformly being spread in alloy material Upper one layer of RJ2 melting coverture, additional amount are the 1.5% of weight alloy.Continue to heat, is warming up to 750 DEG C to temperature, furnace charge is complete After running down, 15 min are stood, remove surface slag, is uniformly sprinkled in bath surface and accounts for the RJ2 covering that weight alloy is 0.05% Agent obtains cleaner alloy molten solution.
(6) temperature of melt obtained by step (5) is adjusted to after 650 DEG C, step (4) preheated coating zinc oxide is added Graphene-aluminium block body green compact, after fusing, temperature rises to 800 DEG C of melting 30min and obtains Composite Melt.
(7) after Composite Melt temperature obtained by step (6) being down to 600 DEG C, under argon gas protection, importing power is The ultrasonic wave of 1000W, ultrasonic disperse handle 20min, obtain the uniform Composite Melt of coating zinc oxide graphene dispersion.
(8) Composite Melt temperature obtained by step (7) is adjusted to 630 DEG C, removes surface slag, sprinkles a small amount of covering Agent after standing 10min, pours into the steel die that temperature is 200 DEG C, and obtaining content is 3.0wt.% coating zinc oxide graphene The AZ91 magnesium-based composite material of enhancing.
Mechanics Performance Testing, Vickers hardness 65-89HV are carried out to the composite material, yield strength reaches 156- 180MPa, elongation percentage reach 7.8-9.5%, are a kind of more good composite materials of mechanical property.
Fig. 1 is coating zinc oxide graphene SEM pattern used in the present invention.It is uniform that flake graphite alkene surface can be observed in figure Be coated with one layer of Zinc oxide nanoparticle.
Fig. 2 is AZ91 alloy microscopic structure prepared by the present invention.Show that crystallite dimension is about 90 μm in figure.
Fig. 3 is that the content prepared under the conditions of the embodiment of the present invention 1 is that 0.1wt.% coating zinc oxide graphene enhances AZ91 magnesium-based composite material microscopic structure.It is shown in figure, which is about 50 μm, and grain refining effect is brighter It is aobvious.

Claims (1)

1. a kind of method of coating zinc oxide graphene enhancing composite material of magnesium alloy, it is characterized in that the following steps are included:
(1) coating zinc oxide graphene is pre-dispersed: press 1-5g/L concentration ratio, by coating zinc oxide graphene be added to ethyl alcohol or In distilled water, ultrasonic 0.5-2h obtains finely dispersed Dispersion of Reinforcement liquid;
(2) ratio for being 10-25: 90-75 in coating zinc oxide graphene and the mass ratio of pure aluminium powder, by granularity less than 400 mesh Pure aluminium powder be added in dispersion liquid obtained by step (1), obtain coating zinc oxide graphene-after ultrasound and mechanical stirring 0.5-2h The uniformly mixed slurries of aluminium powder;
(3) after to the filtering of slurries obtained by step (2), then vacuum dried to obtain coating zinc oxide graphene-aluminium powder pre-dispersed Even mixed-powder;
(4) by mixed-powder obtained by step (3), it is pre-dispersed relatively that coating zinc oxide graphene is made using 300-600MPa pressure Even block green compact, be then preheated to 60-100 DEG C it is spare;
(5) prepared by composite material of magnesium alloy: accounting for composite material gross mass by coating zinc oxide graphene addition quality is 0.1-5% Magnesium alloy material, add it in crucible, heat, while uniformly sprinkling one layer of RJ2 melting coverture in alloy material, Additional amount is the 0.5-1.5% of magnesium alloy weight;Continue to heat, is warming up to 650-750 DEG C, after furnace charge is completely melt to temperature, it is quiet 5-15 min is set, surface slag is removed, is uniformly sprinkled in bath surface and accounts for the RJ2 coverture that weight alloy is 0.05-0.1%, obtained Obtain magnesium alloy melt;
(6) temperature of magnesium alloy melt obtained by step (5) is adjusted to after 550-650 DEG C, step (4) preheated cladding is added Zinc oxide graphene-aluminium block body green compact, after fusing, temperature rises to 700-800 DEG C of melting 5-30min and obtains Composite Melt;
(7) after Composite Melt temperature obtained by step (6) being down to 550-650 DEG C, under argon gas protection, use power for 500- The ultrasonic wave of 1000W, ultrasonic disperse handle 1-20min, obtain the uniform Composite Melt of coating zinc oxide graphene dispersion;
(8) Composite Melt temperature obtained by step (7) is adjusted to 550-630 DEG C, removes surface slag, it is uniform in bath surface The RJ2 coverture for accounting for that weight alloy is 0.05-0.1% is sprinkled, after standing 1-10min, pours into the steel that temperature is 100-200 DEG C In mold, the magnesium-based composite material of coating zinc oxide graphene enhancing is obtained.
CN201811104028.4A 2018-09-21 2018-09-21 Method for reinforcing magnesium alloy composite material by coating zinc oxide graphene Active CN109266893B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110453113A (en) * 2019-09-16 2019-11-15 宜春学院 A kind of method of cesium oxide modified graphene enhancing Al alloy composite
CN115747594A (en) * 2022-12-27 2023-03-07 宜春学院 Method for modifying carbon nano tube reinforced magnesium matrix composite material by using mace structure

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CN104894419B (en) * 2015-02-26 2017-01-04 南昌大学 A kind of coated magnesium oxide Graphene strengthens the method for magnesium base composite material
CN106893881A (en) * 2017-03-28 2017-06-27 宜春学院 A kind of method that zirconium oxide modified graphene strengthens magnesium base composite material
US20170268088A1 (en) * 2014-02-21 2017-09-21 Terves Inc. High Conductivity Magnesium Alloy
CN107267826A (en) * 2017-05-16 2017-10-20 苏州莱特复合材料有限公司 A kind of modified graphene enhancing magnesium-base metal material and preparation method thereof
CN107282134A (en) * 2016-04-12 2017-10-24 中国科学院上海硅酸盐研究所 A kind of ZnO photocatalyst of graphene coated and preparation method thereof

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US20170268088A1 (en) * 2014-02-21 2017-09-21 Terves Inc. High Conductivity Magnesium Alloy
CN104894419B (en) * 2015-02-26 2017-01-04 南昌大学 A kind of coated magnesium oxide Graphene strengthens the method for magnesium base composite material
CN107282134A (en) * 2016-04-12 2017-10-24 中国科学院上海硅酸盐研究所 A kind of ZnO photocatalyst of graphene coated and preparation method thereof
CN106893881A (en) * 2017-03-28 2017-06-27 宜春学院 A kind of method that zirconium oxide modified graphene strengthens magnesium base composite material
CN107267826A (en) * 2017-05-16 2017-10-20 苏州莱特复合材料有限公司 A kind of modified graphene enhancing magnesium-base metal material and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110453113A (en) * 2019-09-16 2019-11-15 宜春学院 A kind of method of cesium oxide modified graphene enhancing Al alloy composite
CN115747594A (en) * 2022-12-27 2023-03-07 宜春学院 Method for modifying carbon nano tube reinforced magnesium matrix composite material by using mace structure
CN115747594B (en) * 2022-12-27 2023-05-16 宜春学院 Method for reinforcing magnesium-based composite material by using spike rod structure modified carbon nano tube

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