CN106834776B - Ni graphenes heteromers strengthen the preparation method of 6061 alloy-base composite materials - Google Patents

Ni graphenes heteromers strengthen the preparation method of 6061 alloy-base composite materials Download PDF

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CN106834776B
CN106834776B CN201611174172.6A CN201611174172A CN106834776B CN 106834776 B CN106834776 B CN 106834776B CN 201611174172 A CN201611174172 A CN 201611174172A CN 106834776 B CN106834776 B CN 106834776B
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graphenes
heteromers
alloy
preparation
graphene
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CN106834776A (en
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何春年
刘光
赵乃勤
师春生
刘恩佐
何芳
李群英
李家俊
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Tianjin University
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Tianjin 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
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17Metallic particles coated with metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0084Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Powder Metallurgy (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention, which provides a kind of Ni graphenes heteromers, strengthens the preparation method of 6061 alloy-base composite materials, including:Nickelous nitrate hexahydrate, glucose, sodium chloride are well mixed in deionized water according to certain quality proportioning, Freeze Drying Technique is used to well mixed solution, obtain precursor powder, utilize chemical vapor deposition, calcining reduction, sodium chloride template is finally washed with deionized water and obtains Ni graphene heteromers;The Ni graphenes heteromers of acquisition and 6061 alloyed powders are put into ball grinder, full of argon gas as protective atmosphere after vacuumizing;By intermittent mechanical milling process, the alloy-based composite powder of Ni graphenes/6061 is made.The hot pressing under the conditions of vacuum hotpressing by the composite powder of gained, obtains the block composite material of Ni graphene/6061.The alloy-base composite material of obtained Ni graphenes of the present invention/6061 has the advantages of mechanical property is good.

Description

Ni- graphenes heteromers strengthen the preparation method of 6061 alloy-base composite materials
Technical field:
The present invention relates to a kind of preparation method for improving 6061 alloy-base composite material mechanical properties, belong to powder metallurgy skill Art field.
Background technology:
6061 alloys have higher mechanical property, specific strength, are widely used in the life such as building, aircraft, automobile always In every field.As requirement of the modern science and technology to structural material improves constantly, 6061 simple alloy materials are difficult full For sufficient modern industry for the application requirement of high-strength light, it is that one kind realizes that these will that graphene, which strengthens 6061 alloy-base composite materials, The ideal material asked.
Graphene has higher mechanical property, single layer of carbon atom as the enhancing phase gradually to attract attention in the last few years Graphene be the stiff materials the most found so far.Strengthen grinding for 6061 alloy-base composite materials for graphene at present Study carefully mainly by graphene and 6061 powder mixing high-energy ball millings, be molded into block materials, the process of this high-energy ball milling for The destruction of graphene seriously reduces the enhancing effect of graphene than more serious, and not moistening due to graphene and aluminum substrate Moisture performance, cause the interface bond strength of final composite weaker, interface load transmission is less efficient, and this is that graphene increases Where the bottleneck that strong 6061 alloy-base composite material runs into, how to keep realizing well on the basis of graphene-structured is complete Scattered and strong clean interface cohesion is the focus studied at present.
The content of the invention:
It is an object of the invention to provide the preparation side that a kind of Ni- graphenes heteromers strengthen 6061 alloy-base composite materials Method, strengthen the combination of 6061 alloy-base composite material median surfaces not using nickel-loaded metallic particles on graphene so as to improve graphene The problem of firm, realize the raising of 6061 alloy substrate mechanical properties.To achieve the above object, the present invention is by following technology What scheme was realized,
A kind of Ni- graphenes heteromers strengthen the preparation method of 6061 alloy-base composite materials, including following step:
(1) preparation of Ni- graphenes heteromers:By Nickelous nitrate hexahydrate, glucose, sodium chloride according to 0.5~2:1~5: 40~60 quality proportioning is well mixed in deionized water, Freeze Drying Technique is used to well mixed solution, before acquisition Body powder is driven, using chemical vapor deposition, calcining reduction, sodium chloride template is finally washed with deionized water and obtains Ni- graphenes Heteromers.
(2) preparation of the alloy-based composite powder of Ni- graphenes/6061:The Ni- graphenes heteromers of acquisition and 6061 are closed Bronze is according to mass ratio 1:50~300 ratio is put into ball grinder, full of argon gas as protective atmosphere after vacuumizing;By Intermittent mechanical milling process, the alloy-based composite powder of Ni- graphenes/6061 is made.
(3) composite powder of gained is placed in 560-600 DEG C, hot pressing under the conditions of 40-50MPa vacuum hotpressing, obtains Ni- The block composite material of graphene/6061.
Can be with step (2):By the halfhour mechanical milling process of the interval of every ball milling ten minutes, be made Ni- graphenes/ 6061 alloy-based composite powders.
The present invention is prepared for the composite of Ni- graphenes heteromers/6061 using salt template and powder metallurgic method, utilizes The nickel metal nanoparticle loaded on graphene generates intermetallic compound to improve in recombination process with aluminium base precursor reactant Non-wetted present situation between aluminium and carbon, improves interfacial bonding property, and realizes the reinforcing to 6061 matrixes, for high-strength light Application of the alloy material of matter 6061 in structural material has preferable prospect.
Brief description of the drawings:
Fig. 1 is the Ni- graphene heteromers scanned photographs obtained by the embodiment of the present invention 2.
Fig. 2 be the interval ball milling of the embodiment of the present invention 2 it is complete obtained by the scanning of the composite powder of Ni- graphenes heteromers/6061 Photo.
Fig. 3 is the metallographic structure photo of the composite of Ni- graphenes/6061 obtained by the embodiment of the present invention 2.
Fig. 4 is that the aluminium carbon interface of the composite of Ni- graphenes/6061 obtained by the embodiment of the present invention 2 transmits photo.
Fig. 5 is the embodiment of the present invention 1, and the composite tensile sample of Ni- graphenes heteromers obtained by 2,3/6061 is set Meter figure.
Fig. 6 is the stress strain curve figure of the composite of Ni- graphenes/6061 obtained by the embodiment of the present invention 2.
Embodiment:
The present invention prepares the heteromers of uniform load Ni nano particles on high-quality graphene using salt template first, then It is mixed with 6061 alloyed powders of 45 μm of particle diameters, using ten minutes halfhour ball-milling technologies of interval of every ball milling, with protection The structure of graphene, finally using 600 DEG C, 45MPa vacuum hotpressing condition progress is hot-forming.Utilize what is loaded on graphene Ni nano particles, by forming Al3Ni intermetallic compounds improve aluminium and the non-wetted present situation of carbon in forming process, so as to change Kind interface cohesion, improve the mechanical property of 6061 alloys.
The present invention is further illustrated with reference to specific embodiment, is not intended to limit the present invention.
Embodiment 1
(1) that 1.2g Nickelous nitrate hexahydrates, 2.05g glucose, 40g sodium chloride are placed in into magnetic agitation 6 in deionized water is small When, the mixed solution of gained is placed in 48h in refrigerator, the solution for freezing real is placed in freeze drier and is freeze-dried 24h, is obtained Presoma composite powder;The presoma composite powder of gained is placed in 750 DEG C, calcining 2 hours, last water are reduced in argon nitrogen atmosphere Wash:Remove sodium chloride and obtain Ni- graphene heteromers, as shown in Figure 1.
(2) by the Ni- graphene heteromers of gained according to 1:199 ratio is placed in ball grinder, is filled with argon gas as guarantor Protect atmosphere.In planetary ball mill by low speed in short-term interval ball milling (360 revs/min, per ball milling 10min interval 90min, ball Grind 90min).
(3) composite powder obtained by is placed in 580 DEG C, hot pressing one hour under the conditions of 45MPa vacuum hotpressing, obtains Ni- stones The block composite material of black alkene/6061.
(4) sample obtained in (3) is prepared into tensile sample, tensile sample design is as shown in Figure 5.
Tensile strength of the composite of prepared high-performance Ni- graphenes of this experiment/6061 under hot pressing state is 188Mpa, elongation percentage 25.5%
Embodiment 2
(1) that 1.2g Nickelous nitrate hexahydrates, 2.05g glucose, 40g sodium chloride are placed in into magnetic agitation 6 in deionized water is small When, the mixed solution of gained is placed in 48h in refrigerator, the solution for freezing real is placed in freeze drier and is freeze-dried 24h, is obtained Presoma composite powder;The presoma composite powder of gained is placed in 750 DEG C, calcining 2 hours, last water are reduced in argon nitrogen atmosphere Wash:Remove sodium chloride and obtain Ni- graphene heteromers, as shown in Figure 1.
(2) by the Ni- graphene heteromers of gained according to 1:150 ratio is placed in ball grinder, is filled with argon gas as guarantor Protect atmosphere.In planetary ball mill by low speed in short-term interval ball milling (360 revs/min, per ball milling 10min interval 90min, ball Grind 90min), resulting composite powder is as shown in Figure 2.
(3) composite powder obtained by is placed in 580 DEG C, hot pressing one hour under the conditions of 45MPa vacuum hotpressing, obtains Ni- stones The block composite material of black alkene/6061, its metallograph is as shown in figure 3, interface analysis transmission plot is as shown in Figure 4.
(4) sample obtained in (3) is prepared into tensile sample, tensile sample design is as shown in Figure 5.
Tensile strength of the composite of prepared high-performance Ni- graphenes of this experiment/6061 under hot pressing state is 213Mpa, elongation percentage 23.4%, as shown in Figure 6.
Embodiment 3
(1) that 1.2g Nickelous nitrate hexahydrates, 2.05g glucose, 40g sodium chloride are placed in into magnetic agitation 6 in deionized water is small When, the mixed solution of gained is placed in 48h in refrigerator, the solution for freezing real is placed in freeze drier and is freeze-dried 24h, is obtained Presoma composite powder;The presoma composite powder of gained is placed in 750 DEG C, calcining 2 hours, last water are reduced in argon nitrogen atmosphere Wash:Remove sodium chloride and obtain Ni- graphene heteromers, as shown in Figure 1.
(2) by the Ni- graphene heteromers of gained according to 1:99 ratio is placed in ball grinder, is filled with argon gas as protection Atmosphere.In planetary ball mill by low speed in short-term interval ball milling (360 revs/min, per ball milling 10min interval 90min, ball milling 90min)。
(3) composite powder obtained by is placed in 580 DEG C, hot pressing one hour under the conditions of 45MPa vacuum hotpressing, obtains Ni- stones The block composite material of black alkene/6061.
(4) sample obtained in (3) is prepared into tensile sample, tensile sample design is as shown in Figure 5.
Tensile strength of the composite of prepared high-performance Ni- graphenes of this experiment/6061 under hot pressing state is 200Mpa, elongation percentage 18%.

Claims (1)

1. a kind of Ni- graphenes heteromers strengthen the preparation method of 6061 alloy-base composite materials, including following step:
(1) preparation of Ni- graphenes heteromers:By Nickelous nitrate hexahydrate, glucose, sodium chloride according to 0.5~2:1~5:40~ 60 quality proportioning is well mixed in deionized water, is used Freeze Drying Technique to well mixed solution, is obtained presoma Powder, using chemical vapor deposition, calcining reduction, it is heteromeric that sodium chloride template acquisition Ni- graphenes are finally washed with deionized water Body;
(2) preparation of the alloy-based composite powder of Ni- graphenes/6061:By the Ni- graphenes heteromers and 6061 alloyed powders of acquisition According to mass ratio 1:50~300 ratio is put into ball grinder, full of argon gas as protective atmosphere after vacuumizing, by every ball Ten minutes halfhour mechanical milling processes of interval of mill, the alloy-based composite powder of Ni- graphenes/6061 is made;
(3) composite powder of gained is placed in 580 DEG C, hot pressing one hour under the conditions of 45MPa vacuum hotpressing, obtains Ni- graphite The block composite material of alkene/6061.
CN201611174172.6A 2016-12-16 2016-12-16 Ni graphenes heteromers strengthen the preparation method of 6061 alloy-base composite materials Expired - Fee Related CN106834776B (en)

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CN107460375A (en) * 2017-07-21 2017-12-12 天津大学 A kind of method of improvement Ni graphene heteromers reinforced aluminum matrix composites mechanical properties
CN107538016A (en) * 2017-07-28 2018-01-05 天津大学 A kind of method for the interface wellability for improving graphene and fine aluminium
CN107794396A (en) * 2017-09-22 2018-03-13 天津大学 A kind of preparation method of Cu graphenes heteromers reinforced aluminum matrix composites
CN109482865A (en) * 2018-09-12 2019-03-19 天津大学 A method of high-content graphene nanometer sheet/carbon/carbon-copper composite material is prepared in situ
CN110918978B (en) * 2019-12-16 2022-04-19 哈尔滨工程大学 Reinforcing phase reinforced composite powder with functional layer for use in fusing technology, and preparation method and application thereof
CN115466459B (en) * 2022-09-06 2024-02-27 成都航空职业技术学院 Modified polypropylene fused deposition molding granule and preparation method thereof

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CN105861865A (en) * 2016-06-03 2016-08-17 南昌航空大学 Method for preparing graphene reinforced aluminum matrix composite material by microwave sintering

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CN105112699A (en) * 2015-06-25 2015-12-02 中国航空工业集团公司北京航空材料研究院 Preparation method of graphene/aluminum alloy composite material
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