WO2020000615A1 - Matériau composite métallique - Google Patents

Matériau composite métallique Download PDF

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Publication number
WO2020000615A1
WO2020000615A1 PCT/CN2018/101941 CN2018101941W WO2020000615A1 WO 2020000615 A1 WO2020000615 A1 WO 2020000615A1 CN 2018101941 W CN2018101941 W CN 2018101941W WO 2020000615 A1 WO2020000615 A1 WO 2020000615A1
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Prior art keywords
ball milling
mixed powder
powder
metal composite
ball
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PCT/CN2018/101941
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English (en)
Chinese (zh)
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樊璠
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樊璠
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Priority to US16/765,180 priority Critical patent/US20200347482A1/en
Priority to US16/560,962 priority patent/US20200002786A1/en
Publication of WO2020000615A1 publication Critical patent/WO2020000615A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-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
    • C22C32/0084—Non-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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/05—Light metals
    • B22F2301/058—Magnesium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/40—Carbon, graphite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/40—Carbon, graphite
    • B22F2302/403—Carbon nanotube
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C22C2026/002—Carbon nanotubes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/04—Hydrogen absorbing

Definitions

  • the invention relates to the technical field of new energy materials, in particular to a green metal composite material.
  • the amount of adsorption is also relatively low, between about 3-6 wt%, and the conditions are harsh, the temperature is 78K, and the pressure is 40bars.
  • activated carbon is cheap and easily available. If proper methods can be used to improve its performance, it has great application prospects.
  • the activated carbon is treated with nitric acid or NaOCl, and its hydrogen absorption amount and discharge amount when used as an electrode are significantly improved.
  • the reason why carbon nanotubes and nano-carbon fibers have become a popular hydrogen storage material is that their large hydrogen storage capacity generally reaches 10% by weight, and some even reach more than 60% by weight. But some scientists have tested this before, but it ended in failure.
  • the purpose of the present invention is to provide a green metal composite material, thereby overcoming the disadvantages of the prior art.
  • the present invention provides a green metal composite material, which is characterized in that the green metal composite material is prepared by the following method: providing Mg, Mo, Al, Ni, and Ti powder; according to a predetermined chemical formula, the Mg, Mo, Al, Ni, and Ti powders were weighed; Mg, Mo, Al, Ni, and Ti powders were weighed first to obtain a first mixed powder; and the first mixed powder was vacuum smelted to obtain a Mg-based alloy Ingots; crushing Mg-based alloy ingots; providing carbon nanotubes and graphene powders; surface modification of carbon nanotubes and graphene powders; crushing Mg-based alloy ingots and surface-modified carbon nanotubes and The graphene powder is mixed and subjected to a second ball milling to obtain a second mixed powder; the second mixed powder is subjected to a first heat treatment to obtain a third mixed powder; and the third mixed powder is subjected to a second hot-press sintering.
  • the first ball milling of Mg, Mo, Al, Ni, and Ti powders after the symmetrical weighting is specifically: the ball milling atmosphere is an argon atmosphere, the ball milling speed is 1500-1800r / min, and the ball milling time is 10- In 20h, the ball-to-material ratio is 8: 1-9: 1.
  • the ball milling atmosphere is an argon atmosphere
  • the ball milling speed is 1500-1800r / min
  • the ball milling time is 10-
  • the ball-to-material ratio is 8: 1-9: 1.
  • each ball is milled for 60-70min, and the ball milling is suspended for 4-5min.
  • the temperature in the ball mill tank is controlled below 600 ° C.
  • the vacuum melting of the first mixed powder is specifically: the vacuum degree is lower than 0.01 Pa, the melting time is 80-100 min, and the alloy ingot is inverted once every 200-250 s during the melting process.
  • the surface modification of the carbon nanotubes and the graphene powder is specifically: disposing an organic solvent of a silane coupling agent, wherein the weight percentage of the silane coupling agent is 2-3 wt%; And the graphene powder are placed in an organic solution of a silane coupling agent and stirred, the stirring time is 50-70 min, and the stirring temperature is 70-80 ° C.
  • the second ball milling is specifically: the ball milling atmosphere is an argon atmosphere, the ball milling speed is 500-600r / min, the ball milling time is 5-8h, and the ball-to-material ratio is 4: 1-5: 1.
  • the ball milling atmosphere is an argon atmosphere
  • the ball milling speed is 500-600r / min
  • the ball milling time is 5-8h
  • the ball-to-material ratio is 4: 1-5: 1.
  • each ball is milled for 30-40 minutes, and the ball milling is suspended for 4-5 minutes.
  • the temperature in the ball mill tank is controlled below 300 ° C.
  • the second mixed powder 100-120 parts of Mg-based alloy ingots after crushing, 10-20 parts of carbon nanotubes after surface modification, and surface modification are included in terms of parts by weight.
  • the latter graphene powder accounts for 3-5 parts.
  • the first heat treatment of the second mixed powder is specifically: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 600-650 ° C, the heat treatment time is 10-20min, and the heating rate is 10-20 ° C / min.
  • the second hot-pressing sintering of the third mixed powder is specifically: the hot-pressing air pressure is lower than 0.03Pa, the hot-pressing temperature is 700-780 ° C, the hot-pressing pressure is 5-10MPa, and the hot-pressing time For 5-10min.
  • Mg-based hydrogen storage materials Compared with coordinated hydride hydrogen storage materials, Mg-based hydrogen storage materials have more stable chemical properties, can adapt to more severe use environments, and have more material storage requirements. Loose, lower storage costs. Compared with rare-earth hydrogen storage materials, Mg-based hydrogen storage materials do not include important rare-earth elements, and they have a wide range of raw materials and are not easily controlled by other countries. However, for Mg-based hydrogen storage materials, the biggest problem is that the hydrogen storage capacity is weak. At the same time, the modification of Mg-based hydrogen storage materials and the improvement of hydrogen storage capacity by doping metal elements have actually reached the theory. At the limit, hydrogen storage capacity can no longer be improved by simple composition design.
  • the process of the present invention well solves the problem of poor compatibility of non-metal particles and metal substrates, easy segregation, With the problem of unstable nature, a hydrogen storage material with stable properties, strong hydrogen storage capacity, and suitable for industrial production was prepared at a lower cost.
  • Green metal composite materials are prepared by the following methods: providing Mg, Mo, Al, Ni, and Ti powder; weighing Mg, Mo, Al, Ni, and Ti powder according to a predetermined chemical formula; Mg, Mo, and Al, Ni, and Ti powders are subjected to a first ball milling to obtain a first mixed powder; the first mixed powder is vacuum smelted to obtain an Mg-based alloy ingot; the Mg-based alloy ingot is crushed; carbon nanotubes and graphene powder are provided; Carbon nanotubes and graphene powders are subjected to surface modification; the broken Mg-based alloy ingots and surface-modified carbon nanotubes and graphene powders are mixed and subjected to a second ball milling to obtain a second mixed powder; The mixed powder is subjected to a first heat treatment to obtain a third mixed powder; the third mixed powder is subjected to a second hot-pressing sintering.
  • the first ball milling of Mg, Mo, Al, Ni, and Ti powders after symmetrical weighting is as follows: the ball milling atmosphere is argon, the ball milling speed is 1500r / min, the ball milling time is 10h, and the ball-to-material ratio is 8: 1. In the process, each ball was milled for 60 minutes, and the ball milling was suspended for 4 minutes. During the ball milling, the temperature in the ball mill tank was controlled below 600 ° C.
  • the vacuum melting of the first mixed powder is specifically: the vacuum degree is less than 0.01 Pa, and the melting time is 80 min. In the melting process, the alloy ingot is inverted once every 200 s of melting.
  • the surface modification of the carbon nanotubes and graphene powder is specifically: disposing an organic solvent of a silane coupling agent, wherein the weight percentage of the silane coupling agent is 2% by weight; placing the carbon nanotubes and graphene powder on the silane coupling agent And stir in the organic solution, the stirring time is 50 min, and the stirring temperature is 70 ° C.
  • the second ball milling is specifically: the ball milling atmosphere is an argon atmosphere, the ball milling speed is 500 r / min, the ball milling time is 5 h, the ball-to-material ratio is 4: 1, during the ball milling process, each ball milling is 30 minutes, and the ball milling is suspended for 4 minutes.
  • the temperature in the tank was below 300 ° C.
  • 100 parts by weight of the broken Mg-based alloy ingot, 10 parts by surface-modified carbon nanotubes, and 3 parts by surface-modified graphene powder are calculated in terms of parts by weight.
  • Green metal composite materials are prepared by the following methods: providing Mg, Mo, Al, Ni, and Ti powder; weighing Mg, Mo, Al, Ni, and Ti powder according to a predetermined chemical formula; Mg, Mo, and Al, Ni, and Ti powders are subjected to a first ball milling to obtain a first mixed powder; the first mixed powder is vacuum smelted to obtain an Mg-based alloy ingot; the Mg-based alloy ingot is crushed; carbon nanotubes and graphene powder are provided; Carbon nanotubes and graphene powders are subjected to surface modification; the broken Mg-based alloy ingots and surface-modified carbon nanotubes and graphene powders are mixed and subjected to a second ball milling to obtain a second mixed powder; The mixed powder is subjected to a first heat treatment to obtain a third mixed powder; the third mixed powder is subjected to a second hot-pressing sintering.
  • the first ball milling of Mg, Mo, Al, Ni, and Ti powders after symmetrical weighting is as follows: the ball milling atmosphere is argon, the ball milling speed is 1800r / min, the ball milling time is 20h, and the ball-to-material ratio is 9: 1.
  • each ball was milled for 70 minutes, and the milling was suspended for 5 minutes.
  • the temperature in the ball mill tank was controlled below 600 ° C.
  • the vacuum melting of the first mixed powder is specifically: the vacuum degree is less than 0.01 Pa, and the melting time is 100 minutes. In the melting process, the alloy ingot is inverted once every 250 s of melting.
  • the surface modification of carbon nanotubes and graphene powder is specifically: disposing an organic solvent of a silane coupling agent, wherein the weight percentage of the silane coupling agent is 3% by weight; placing the carbon nanotubes and graphene powder on the silane coupling agent The organic solution was stirred in the organic solution for 70 minutes, and the stirring temperature was 80 ° C.
  • the second ball milling is specifically: the ball milling atmosphere is an argon atmosphere, the ball milling speed is 600r / min, the ball milling time is 8h, the ball-to-material ratio is 5: 1, during the ball milling process, each ball milling is 40min, the ball milling is suspended for 5min, and the ball milling process is controlled
  • the temperature in the tank was below 300 ° C.
  • the first heat treatment of the second mixed powder is specifically: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 650 ° C., the heat treatment time is 20 minutes, and the heating rate is 20 ° C./min.
  • the second hot-pressing sintering of the third mixed powder is specifically: the hot-pressing air pressure is less than 0.03 Pa, the hot-pressing temperature is 780 ° C., the hot-pressing pressure is 10 MPa, and the hot-pressing time is 10 min.
  • the green metal composite is prepared by the following methods: providing Mg, Mo, Al, Ni, and Ti powder; weighing Mg, Mo, Al, Ni, and Ti powder according to a predetermined chemical formula; Mg, Mo, and Al, Ni, and Ti powders are subjected to a first ball milling to obtain a first mixed powder; the first mixed powder is vacuum smelted to obtain an Mg-based alloy ingot; the Mg-based alloy ingot is crushed; carbon nanotubes and graphene powder are provided; Carbon nanotubes and graphene powders are subjected to surface modification; the broken Mg-based alloy ingots and surface-modified carbon nanotubes and graphene powders are mixed and subjected to a second ball milling to obtain a second mixed powder; The mixed powder is subjected to a first heat treatment to obtain a third mixed powder; the third mixed powder is subjected to a second hot-pressing sintering.
  • the first ball milling of Mg, Mo, Al, Ni, and Ti powders after symmetrical weighting is as follows: the ball milling atmosphere is argon, the ball milling speed is 1600r / min, the ball milling time is 15h, and the ball-to-material ratio is 8.5: 1.
  • each ball was milled for 65 minutes, and the ball mill was suspended for 4.5 minutes.
  • the temperature in the ball mill tank was controlled below 600 ° C.
  • the vacuum melting of the first mixed powder is specifically: the vacuum degree is less than 0.01 Pa, and the melting time is 90 minutes. During the melting process, the alloy ingot is inverted once every 220 s of melting.
  • the surface modification of carbon nanotubes and graphene powder is specifically: disposing an organic solvent of a silane coupling agent, wherein the weight percentage of the silane coupling agent is 2.5% by weight; placing the carbon nanotubes and graphene powder in a silane coupling The organic solution of the agent was stirred, and the stirring time was 60 min, and the stirring temperature was 75 ° C.
  • the second ball milling is specifically: the ball milling atmosphere is an argon atmosphere, the ball milling speed is 550r / min, the ball milling time is 6h, the ball-to-material ratio is 4.5: 1, during the ball milling process, each ball milling is 35min, the ball milling is suspended for 4.5min, and the ball milling process is controlled
  • the temperature in the ball mill tank is below 300 ° C.
  • the first heat treatment of the second mixed powder is specifically: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 620 ° C., the heat treatment time is 15 minutes, and the heating rate is 15 ° C./min.
  • the second hot-pressing sintering of the third mixed powder is specifically: the hot-pressing air pressure is lower than 0.03 Pa, the hot-pressing temperature is 730 ° C, the hot-pressing pressure is 8 MPa, and the hot-pressing time is 8 min.
  • Green metal composite materials are prepared by the following methods: providing Mg, Mo, Al, Ni, and Ti powder; weighing Mg, Mo, Al, Ni, and Ti powder according to a predetermined chemical formula; Mg, Mo, and Al, Ni, and Ti powders are subjected to a first ball milling to obtain a first mixed powder; the first mixed powder is vacuum smelted to obtain an Mg-based alloy ingot; the Mg-based alloy ingot is crushed; carbon nanotubes and graphene powder are provided; Carbon nanotubes and graphene powders are subjected to surface modification; the broken Mg-based alloy ingots and surface-modified carbon nanotubes and graphene powders are mixed and subjected to a second ball milling to obtain a second mixed powder; The mixed powder is subjected to a first heat treatment to obtain a third mixed powder; the third mixed powder is subjected to a second hot-pressing sintering.
  • the first ball milling of Mg, Mo, Al, Ni, and Ti powder after symmetrical weighting is as follows: the ball milling atmosphere is argon, the ball milling speed is 2000r / min, the ball milling time is 25h, and the ball-to-material ratio is 10: 1. In the process, each ball was milled for 80 minutes, and the ball milling was suspended for 10 minutes. During the ball milling, the temperature in the ball mill tank was controlled below 600 ° C.
  • the vacuum melting of the first mixed powder is specifically: the vacuum degree is less than 0.01 Pa, and the melting time is 90 minutes. During the melting process, the alloy ingot is inverted once every 220 s of melting.
  • the surface modification of carbon nanotubes and graphene powder is specifically: disposing an organic solvent of a silane coupling agent, wherein the weight percentage of the silane coupling agent is 2.5% by weight; placing the carbon nanotubes and graphene powder in a silane coupling The organic solution of the agent was stirred, and the stirring time was 60 min, and the stirring temperature was 75 ° C.
  • the second ball milling is specifically: the ball milling atmosphere is an argon atmosphere, the ball milling speed is 550r / min, the ball milling time is 6h, the ball-to-material ratio is 4.5: 1, during the ball milling process, each ball milling is 35min, the ball milling is suspended for 4.5min, and the ball milling process is controlled
  • the temperature in the ball mill tank is below 300 ° C.
  • the first heat treatment of the second mixed powder is specifically: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 620 ° C., the heat treatment time is 15 minutes, and the heating rate is 15 ° C./min.
  • the second hot-pressing sintering of the third mixed powder is specifically: the hot-pressing air pressure is lower than 0.03 Pa, the hot-pressing temperature is 730 ° C., the hot-pressing pressure is 8 MPa, and the hot-pressing time is 8 min.
  • Green metal composite materials are prepared by the following methods: providing Mg, Mo, Al, Ni, and Ti powder; weighing Mg, Mo, Al, Ni, and Ti powder according to a predetermined chemical formula; Mg, Mo, and Al, Ni, and Ti powders are subjected to a first ball milling to obtain a first mixed powder; the first mixed powder is vacuum smelted to obtain an Mg-based alloy ingot; the Mg-based alloy ingot is crushed; carbon nanotubes and graphene powder are provided; Carbon nanotubes and graphene powders are subjected to surface modification; the broken Mg-based alloy ingots and surface-modified carbon nanotubes and graphene powders are mixed and subjected to a second ball milling to obtain a second mixed powder; The mixed powder is subjected to a first heat treatment to obtain a third mixed powder; the third mixed powder is subjected to a second hot-pressing sintering.
  • the first ball milling of Mg, Mo, Al, Ni, and Ti powders after symmetrical weighting is as follows: the ball milling atmosphere is argon, the ball milling speed is 1600r / min, the ball milling time is 15h, and the ball-to-material ratio is 8.5: 1.
  • each ball was milled for 65 minutes, and the ball mill was suspended for 4.5 minutes.
  • the temperature in the ball mill tank was controlled below 600 ° C.
  • the vacuum melting of the first mixed powder is specifically: the vacuum degree is less than 0.01 Pa, and the melting time is 200 min. In the melting process, the alloy ingot is inverted once every 500 s of melting.
  • the surface modification of carbon nanotubes and graphene powder is specifically: disposing an organic solvent of a silane coupling agent, wherein the weight percentage of the silane coupling agent is 5 wt%; placing the carbon nanotubes and graphene powder on the silane coupling agent The organic solution was stirred in the organic solution for 10 minutes, and the stirring temperature was 20 ° C.
  • the second ball milling is specifically: the ball milling atmosphere is an argon atmosphere, the ball milling speed is 700 r / min, the ball milling time is 10 hours, and the ball-to-material ratio is 8: 1. During the ball milling process, each ball milling is performed for 50 minutes, and the ball milling is suspended for 8 minutes. The temperature in the tank was below 300 ° C. In the second mixed powder, 110 parts by weight of the crushed Mg-based alloy ingots, 15 parts by surface-modified carbon nanotubes, and 4 parts by surface-modified graphene powder.
  • the first heat treatment of the second mixed powder is specifically: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 620 ° C., the heat treatment time is 15 minutes, and the heating rate is 15 ° C./min.
  • the second hot-pressing sintering of the third mixed powder is specifically: the hot-pressing air pressure is lower than 0.03 Pa, the hot-pressing temperature is 730 ° C., the hot-pressing pressure is 8 MPa, and the hot-pressing time is 8 min.
  • Green metal composite materials are prepared by the following methods: providing Mg, Mo, Al, Ni, and Ti powder; weighing Mg, Mo, Al, Ni, and Ti powder according to a predetermined chemical formula; Mg, Mo, and Al, Ni, and Ti powders are subjected to a first ball milling to obtain a first mixed powder; the first mixed powder is vacuum smelted to obtain an Mg-based alloy ingot; the Mg-based alloy ingot is crushed; carbon nanotubes and graphene powder are provided; Carbon nanotubes and graphene powders are subjected to surface modification; the broken Mg-based alloy ingots and surface-modified carbon nanotubes and graphene powders are mixed and subjected to a second ball milling to obtain a second mixed powder; The mixed powder is subjected to a first heat treatment to obtain a third mixed powder; the third mixed powder is subjected to a second hot-pressing sintering.
  • the first ball milling of Mg, Mo, Al, Ni, and Ti powders after symmetrical weighting is as follows: the ball milling atmosphere is argon, the ball milling speed is 1600r / min, the ball milling time is 15h, and the ball-to-material ratio is 8.5: 1.
  • each ball was milled for 65 minutes, and the ball mill was suspended for 4.5 minutes.
  • the temperature in the ball mill tank was controlled below 600 ° C.
  • the vacuum melting of the first mixed powder is specifically: the vacuum degree is less than 0.01 Pa, and the melting time is 90 minutes. During the melting process, the alloy ingot is inverted once every 220 s of melting.
  • the surface modification of carbon nanotubes and graphene powder is specifically: disposing an organic solvent of a silane coupling agent, wherein the weight percentage of the silane coupling agent is 2.5% by weight; placing the carbon nanotubes and graphene powder in a silane coupling The organic solution of the agent was stirred, and the stirring time was 60 min, and the stirring temperature was 75 ° C.
  • the second ball milling is specifically: the ball milling atmosphere is an argon atmosphere, the ball milling speed is 550r / min, the ball milling time is 6h, the ball-to-material ratio is 4.5: 1, during the ball milling process, each ball milling is 35min, the ball milling is suspended for 4.5min, and the ball milling process is controlled
  • the temperature in the ball mill tank is below 300 ° C.
  • the second mixed powder 150 parts by weight of the crushed Mg-based alloy ingot, 5 parts by surface-modified carbon nanotubes, and 1 part by surface-modified graphene powder.
  • the first heat treatment of the second mixed powder is specifically: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 620 ° C., the heat treatment time is 15 minutes, and the heating rate is 15 ° C./min.
  • the second hot-pressing sintering of the third mixed powder is specifically: the hot-pressing air pressure is lower than 0.03 Pa, the hot-pressing temperature is 730 ° C., the hot-pressing pressure is 8 MPa, and the hot-pressing time is 8 min.
  • Green metal composite materials are prepared by the following methods: providing Mg, Mo, Al, Ni, and Ti powder; weighing Mg, Mo, Al, Ni, and Ti powder according to a predetermined chemical formula; Mg, Mo, and Al, Ni, and Ti powders are subjected to a first ball milling to obtain a first mixed powder; the first mixed powder is vacuum smelted to obtain an Mg-based alloy ingot; the Mg-based alloy ingot is crushed; carbon nanotubes and graphene powder are provided; Carbon nanotubes and graphene powders are subjected to surface modification; the broken Mg-based alloy ingots and surface-modified carbon nanotubes and graphene powders are mixed and subjected to a second ball milling to obtain a second mixed powder; The mixed powder is subjected to a first heat treatment to obtain a third mixed powder; the third mixed powder is subjected to a second hot-pressing sintering.
  • the first ball milling of Mg, Mo, Al, Ni, and Ti powders after symmetrical weighting is as follows: the ball milling atmosphere is argon, the ball milling speed is 1600r / min, the ball milling time is 15h, and the ball-to-material ratio is 8.5: 1.
  • each ball was milled for 65 minutes, and the ball mill was suspended for 4.5 minutes.
  • the temperature in the ball mill tank was controlled below 600 ° C.
  • the vacuum melting of the first mixed powder is specifically: the vacuum degree is less than 0.01 Pa, and the melting time is 90 minutes. During the melting process, the alloy ingot is inverted once every 220 s of melting.
  • the surface modification of carbon nanotubes and graphene powder is specifically: disposing an organic solvent of a silane coupling agent, wherein the weight percentage of the silane coupling agent is 2.5% by weight; placing the carbon nanotubes and graphene powder in a silane coupling The organic solution of the agent was stirred, and the stirring time was 60 min, and the stirring temperature was 75 ° C.
  • the second ball milling is specifically: the ball milling atmosphere is an argon atmosphere, the ball milling speed is 550r / min, the ball milling time is 6h, the ball-to-material ratio is 4.5: 1, during the ball milling process, each ball milling is 35min, the ball milling is suspended for 4.5min, and the ball milling process is controlled
  • the temperature in the ball mill tank is below 300 ° C.
  • the first heat treatment of the second mixed powder is specifically: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 700 ° C., the heat treatment time is 25 minutes, and the heating rate is 30 ° C./min.
  • the second hot-pressing sintering of the third mixed powder is specifically: the hot-pressing air pressure is less than 0.03 Pa, the hot-pressing temperature is 820 ° C., the hot-pressing pressure is 20 MPa, and the hot-pressing time is 4 min.

Abstract

L'invention concerne un matériau composite métallique. Le matériau composite métallique est préparé par le procédé suivant : la fourniture de poudres de Mg, Mo, Al, Ni et Ti; le pesage des poudres de Mg, Mo, Al, Ni et Ti selon une formule chimique prédéterminée; la réalisation d'un broyage à boulets en premier temps sur les poudres pesées Mg, Mo, Al, Ni et Ti pour obtenir une première poudre mélangée; la réalisation d'une fusion sous vide sur la première poudre mélangée pour obtenir un lingot d'alliage à base de Mg; le broyage du lingot d'alliage à base de Mg; la fourniture d'un nanotube de carbone et d'une poudre de graphène; la réalisation d'une modification de surface sur le nanotube de carbone et la poudre de graphène; le mélange du lingot d'alliage à base de Mg broyé avec le nanotube de carbone à surface modifiée et la poudre de graphène, et la réalisation d'un broyage à boulets en second temps pour obtenir une seconde poudre mélangée; la réalisation d'un traitement thermique de premier temps sur la seconde poudre mélangée pour obtenir une troisième poudre mélangée; et la réalisation d'un frittage par pressage à chaud en second temps sur la troisième poudre mélangée. Le procédé résout les problèmes de mauvaise compatibilité, de ségrégation facile et de propriétés instables entre des particules non métalliques et une matrice métallique, et prépare un matériau de stockage d'hydrogène qui est stable en termes de propriété, fort dans la capacité de stockage d'hydrogène et approprié pour une production industrielle.
PCT/CN2018/101941 2018-06-29 2018-08-23 Matériau composite métallique WO2020000615A1 (fr)

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Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6958434B2 (ja) * 2018-03-06 2021-11-02 三菱マテリアル株式会社 金属粒子凝集体及びその製造方法並びにペースト状金属粒子凝集体組成物及びこれを用いた接合体の製造方法
CN109364714A (zh) * 2018-11-23 2019-02-22 方雪美 绿色环保汽车尾气清洁剂及其制备方法
CN113695572B (zh) * 2021-08-30 2022-03-11 广东工业大学 一种石墨烯基高熵合金材料的制备方法
CN113862536B (zh) * 2021-09-14 2022-07-08 钢铁研究总院 一种Mg-Al-Y基储氢材料及其制备方法
CN114110420A (zh) * 2021-10-29 2022-03-01 江苏氢枫能源装备有限公司 一种模块化固态储氢单元及制作方法
CN114932225B (zh) * 2022-03-09 2023-09-05 武汉大学 医用3d打印镍钛基复合粉末、制备方法及复合增强材料
CN115106534B (zh) * 2022-08-30 2022-11-18 西安稀有金属材料研究院有限公司 一种多粉末均匀分散的烧结式阳极箔制备方法
CN116237474B (zh) * 2023-02-28 2024-01-02 湖南海创同辉新材料有限公司 一种低碳铌钨合金铸锭的制备方法
CN116043054B (zh) * 2023-03-22 2023-06-16 厦门凯纳石墨烯技术股份有限公司 一种改性石墨烯复合金属材料及其制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1259584A (zh) * 2000-01-20 2000-07-12 南开大学 储氢合金/碳纳米管复合储氢材料
CN1398664A (zh) * 2002-08-28 2003-02-26 武汉理工大学 储氢金属或储氢合金修饰的一维纳米碳储氢材料
CN1900337A (zh) * 2006-07-26 2007-01-24 贵州佑邦科技有限公司 一种四元系镁基储氢合金、其生产方法及应用
CN105170972A (zh) * 2015-09-02 2015-12-23 中南大学 一种Mg-Ti储氢合金粉及其制备方法

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6103024A (en) * 1994-12-22 2000-08-15 Energy Conversion Devices, Inc. Magnesium mechanical alloys for thermal hydrogen storage
BRPI0602153B1 (pt) * 2006-06-06 2017-05-30 Coppe/Ufrj - Coordenação Dos Programas De Pós Graduação De Engenharia Da Univ Fed Do Rio De Janeiro ligas de magnésio para armazenamento reversível de hidrogênio
CN107338381B (zh) * 2017-07-04 2018-11-20 内蒙古科技大学 燃料电池用石墨烯催化的贮氢合金及其制备方法
CN108193107B (zh) * 2017-12-21 2020-04-10 陕西科技大学 一种有机包覆核-壳纳米复合储氢材料的制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1259584A (zh) * 2000-01-20 2000-07-12 南开大学 储氢合金/碳纳米管复合储氢材料
CN1398664A (zh) * 2002-08-28 2003-02-26 武汉理工大学 储氢金属或储氢合金修饰的一维纳米碳储氢材料
CN1900337A (zh) * 2006-07-26 2007-01-24 贵州佑邦科技有限公司 一种四元系镁基储氢合金、其生产方法及应用
CN105170972A (zh) * 2015-09-02 2015-12-23 中南大学 一种Mg-Ti储氢合金粉及其制备方法

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