CN103484706B - Aligned carbon nanotube strengthens device for MMCs and method - Google Patents

Aligned carbon nanotube strengthens device for MMCs and method Download PDF

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CN103484706B
CN103484706B CN201310422144.1A CN201310422144A CN103484706B CN 103484706 B CN103484706 B CN 103484706B CN 201310422144 A CN201310422144 A CN 201310422144A CN 103484706 B CN103484706 B CN 103484706B
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carbon nanotube
crucible
resistance furnace
cushion block
die
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CN103484706A (en
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李贺军
梁军浩
齐乐华
关俊涛
彭斌
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Northwestern Polytechnical University
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Abstract

The invention discloses a kind of aligned carbon nanotube and strengthen device for MMCs and method, being difficult to prepare the technical problem that aligned carbon nanotube strengthens metal-base composites for solving existing preparation facilities.Technical scheme is that the bottom of crucible arranges magnetic stirrer, ultrasonic amplitude bar is equipped with at mouth of pot, crucible is communicated with air pressure tank by the pneumatic tube being provided with reducing valve, and be communicated with die bucket by tubing, be exhausted by installing valvular vapor pipe, crucible and die bucket place the first resistance furnace respectively outward and the second resistance furnace heats, the second resistance furnace outside die bucket places coil outward, utilize punch and upper cushion block sealing die bucket top, utilize shaping die and lower cushion block to carry out sealing die bucket bottom.The present invention utilizes electromagnetic field and ultrasonic wave-coupled to realize dispersed in molten metal of carbon nanotube, and then by induced by magnetic field and stress induced coupling, the aligned carbon nanotube that is shaped strengthens metal-base composites.

Description

Aligned carbon nanotube strengthens device for MMCs and method
Technical field
The present invention relates to a kind of device for MMCs, particularly a kind of aligned carbon nanotube strengthens device for MMCs.Also relate to a kind of this aligned carbon nanotube enhancing device for MMCs that utilizes and prepare the method that aligned carbon nanotube strengthens metal-base composites.
Background technology
Metal-base composites because Young's modulus is high, toughness and shock-resistance is good, gain great popularity to little, the higher advantage such as electroconductibility and thermal conductivity of the susceptibility of temperature change.
General employing fiber C, Ti fiber, fiber B, Al 2o 3staple fibre, SiC whisker, C particle, SiC particle, A1 2o 3particle, B 4c particle, Si 3n 4particle, WC particle, Mo 2c particle, ZrO 2particle, ZrB 2the wild phases such as particle, carbon nanotube and graphite carry out compound and obtain metal-base composites.Wherein carbon nanotube is because of the mechanical property of its excellence, is widely used in the reinforcement of matrix material.Carbon nanotube has very high axial strength and rigidity, and when carbon nanotube is in the base in when aligning, the mechanical property along its arragement direction far above other directions, will show obvious anisotropy.
Document " publication number is the Chinese invention patent of CN102070877A " discloses a kind of ordered arrangement carbon nano tube/epoxy resin composite material and preparation method thereof.The method carbon nanotube used is that at least load has iron, cobalt, the carbon nanotube that nickel and ferriferrous oxide nano-particle are wherein a kind of, first use mechanical stirring and ultrasonic method by the above-mentioned carbon nanotube of 1 ~ 15 mass parts by solvent dispersion in the epoxy resin of 100 mass parts, add the amine curing agent of 10 ~ 50 mass parts after solvent is removed in heating again and mix further, after froth in vacuum, mixture is poured into and is placed in the mould that intensity is the magnetic field of 0.15 ~ 1.0 tesla, after at room temperature solidifying 0.5 ~ 1h, mould is taken out from magnetic field, finally DEG C continuation solidification 4 ~ 24h in room temperature ~ 120.
In prior art, the composite material and preparation method thereof that aligned carbon nanotube strengthens mainly contains stress-induced orientation, electric field induce orientation and induced by magnetic field orientation etc., and technology of preparing in this respect focuses mostly in polymer matrix composite.And to prepare difficulty higher due to it aligned carbon nanotube to be strengthened to the technology of preparing of metal-base composites, domestic and international rarely seen report.This mainly because surface energy that the huge surface of nanometer reinforcement produces make to have nano-scale object between there is extremely strong agglomeration and make particle size become large.How these nanometer reinforcements are dispersed in metallic matrix, and make it ordered arrangement and keep the single body of nano-scale to be prepare the matter of utmost importance that high-performance metal based composites must solve to give full play to its nano effect.
Summary of the invention
Being difficult to prepare the deficiency that aligned carbon nanotube strengthens metal-base composites to overcome existing aligned carbon nanotube enhancing device for MMCs, the invention provides a kind of aligned carbon nanotube and strengthening device for MMCs.This device arranges magnetic stirrer in the bottom of crucible, ultrasonic amplitude bar is equipped with at mouth of pot, crucible is communicated with air pressure tank by the pneumatic tube being provided with reducing valve, and be communicated with die bucket by tubing, be exhausted by installing valvular vapor pipe, crucible and die bucket place the first resistance furnace respectively outward and the second resistance furnace heats, the second resistance furnace outside die bucket places coil outward, utilize punch and upper cushion block sealing die bucket top, utilize shaping die and lower cushion block to carry out sealing die bucket bottom.The present invention utilizes electromagnetic field and ultrasonic wave-coupled to realize dispersed in molten metal of carbon nanotube, then by induced by magnetic field and stress induced coupling, can realize once-forming high performance aligned carbon nanotube and strengthen metal-base composites.
The present invention also provides and utilizes this aligned carbon nanotube enhancing device for MMCs to prepare the method that aligned carbon nanotube strengthens metal-base composites.
The technical solution adopted for the present invention to solve the technical problems is: a kind of aligned carbon nanotube strengthens device for MMCs, is characterized in: comprise reducing valve 1, first resistance furnace 2, air pressure tank 3, crucible 4, magnetic stirrer 5, tubing 6, ultrasonic amplitude bar 7, pneumatic tube 9, punch 10, upper cushion block 11, second resistance furnace 12, vapor pipe 13, valve 14, coil 15, die bucket 16, shaping die 17 and lower cushion block 18.The bottom of crucible 4 is provided with magnetic stirrer 5, ultrasonic amplitude bar 7 is equipped with at mouth of pot 8, crucible 4 is communicated with air pressure tank 3 by the pneumatic tube 9 being provided with reducing valve 1, and be communicated with die bucket 16 by tubing 6, be exhausted by the vapor pipe 13 being provided with valve 14, crucible 4 and die bucket 16 place the first resistance furnace 2 respectively outward and the second resistance furnace 12 heats, the second resistance furnace 12 outside die bucket 16 is outer places coil 15, punch 10 and upper cushion block 11 are used for sealing die bucket 16 top, and shaping die 17 and lower cushion block 18 are used for sealing die bucket 16 bottom.
Utilize above-mentioned aligned carbon nanotube to strengthen device for MMCs and prepare the method that aligned carbon nanotube strengthens metal-base composites, be characterized in comprising the following steps:
Step one, raw metal and carbon nanotube aluminium foil parcel to be loaded in crucible 4, fall punch 10 and compress upper cushion block 11, open reducing valve 1 and valve 14, crucible 4 is communicated with air pressure tank 3, pass into shielding gas by pneumatic tube 9, shielding gas flows through tubing 6, is finally discharged by vapor pipe 13;
Step 2, open the first resistance furnace 2, raw metal in crucible 4 is melted, opens the second resistance furnace 12, preheating die bucket 16 and shaping die 17;
Step 3, until raw metal melt after, open ultrasonic generator, ultrasonic amplitude bar 7 is placed in 5 ~ 10mm place under liquid level, ultrasonic power is 500 ~ 2000W, and ultrasonic frequency is 10 ~ 100kHz, meanwhile, open magnetic stirrer 5, frequency is 2Hz ~ 50Hz, and working current is 10A ~ 1000A, keeps 20-30 minute;
Step 4, taking-up ultrasonic amplitude bar 7, mouth of pot 8 is sealed, blend melt is pressed in die bucket 16 under the influence of air pressure, direct current is passed into coil 15, when melt is cooled to the liquid solid state temperature of material, remove upper cushion block 11 and lower cushion block 18, the descending extruding of punch 10, realize carbon nanotube aligning in metallic matrix, obtain aligned carbon nanotube and strengthen metal-base composites.
The invention has the beneficial effects as follows: this device arranges magnetic stirrer in the bottom of crucible, ultrasonic amplitude bar is equipped with at mouth of pot, crucible is communicated with air pressure tank by the pneumatic tube being provided with reducing valve, and be communicated with die bucket by tubing, be exhausted by installing valvular vapor pipe, crucible and die bucket place the first resistance furnace respectively outward and the second resistance furnace heats, the second resistance furnace outside die bucket places coil outward, utilize punch and upper cushion block sealing die bucket top, utilize shaping die and lower cushion block to carry out sealing die bucket bottom.The present invention utilizes electromagnetic field and ultrasonic wave-coupled to realize dispersed in molten metal of carbon nanotube, then by induced by magnetic field and stress induced coupling, can realize once-forming high performance aligned carbon nanotube and strengthen metal-base composites.
Under ultrasonic wave and induction stirring coupling, can greatly improve the dispersiveness of carbon nanotube in metallic matrix under the prerequisite of decreasing pollution molten metal, and ultrasonic wave can provide energy for surface reaction, improve carbon nanotube and intermetallic wettability.
Compound outfield ultrasonic wave and induction stirring are coupled and disperse to induce to be coupled with compound outfield induced by magnetic field and stress field to induce shaping to combine, and collection dispersion, are oriented to one, can once-forming high-performance metal based composites, and equipment requirements is simple, and cost is low.
The present invention is described in detail below in conjunction with drawings and Examples.
Accompanying drawing explanation
Fig. 1 is the structural representation that aligned carbon nanotube of the present invention strengthens device for MMCs.
In figure, 1-reducing valve, 2-first resistance furnace, 3-air pressure tank, 4-crucible, 5-magnetic stirrer, 6-tubing, 7-ultrasonic amplitude bar, 8-mouth of pot, 9-pneumatic tube, 10-punch, the upper cushion block of 11-, 12-second resistance furnace, 13-vapor pipe, 14-valve, 15-coil, 16 die buckets, 17-shaping die, 18-lower cushion block.
Embodiment
Following examples are with reference to Fig. 1.
Device embodiment.The present invention includes reducing valve 1, first resistance furnace 2, air pressure tank 3, crucible 4, magnetic stirrer 5, tubing 6, ultrasonic amplitude bar 7, pneumatic tube 9, punch 10, upper cushion block 11, second resistance furnace 12, vapor pipe 13, valve 14, coil 15, die bucket 16, shaping die 17 and lower cushion block 18.The bottom of crucible 4 is provided with magnetic stirrer 5, ultrasonic amplitude bar 7 is equipped with at mouth of pot 8, crucible 4 is communicated with air pressure tank 3 by the pneumatic tube 9 being provided with reducing valve 1, and be communicated with die bucket 16 by tubing 6, be exhausted by the vapor pipe 13 being provided with valve 14, crucible 4 and die bucket 16 place the first resistance furnace 2 respectively outward and the second resistance furnace 12 heats, the second resistance furnace 12 outside die bucket 16 is outer places coil 15, utilize punch 10 and upper cushion block 11 to seal die bucket 16 top, utilize shaping die 17 and lower cushion block 18 to carry out sealing die bucket 16 bottom.
Embodiment of the method 1: a kind of method preparing aligned carbon nanotube enhancing magnesium base composite material, comprises the following steps:
Step 1: AZ91D magnesium alloy and the effective Aluminium Foil Package of multi-wall carbon nano-tube are wrapped up in and loads in crucible 4 according to volume fraction 100:1, fall punch 10 and compress cushion block 11, open reducing valve 1 and valve 14, pass into air pressure tank 3, shielding gas is passed into by pneumatic tube 9, flow through tubing 6, finally discharged by vapor pipe 13;
Step 2: open resistance furnace 2, all melts AZ91D magnesium alloy in crucible 4, opens resistance furnace 12, preheating die bucket 16 and shaping die 17;
Step 3: after AZ91D melts, open ultrasonic generator, ultrasonic amplitude bar 7 is placed in 5mm place under liquid level, ultrasonic power is 1500W, ultrasonic frequency is 20kHz, meanwhile, opens magnetic stirrer 5, frequency is 10Hz, and working current is 250A, keeps 20 minutes;
Step 4: take out ultrasonic amplitude bar 7, mouth of pot 8 is sealed, blend melt is pressed in die under the influence of air pressure, direct current is passed into coil 15, when melt is cooled to the liquid solid state temperature 450 DEG C of material, remove cushion block 12 and cushion block 18, punch 10 is descending, utilize high extrusion ratio to extrude, aligned carbon nanotube can be prepared and strengthen AZ91D magnesium base composite material clavate product.
Embodiment of the method 2: a kind of method preparing aligned carbon nanotube reinforced aluminum matrix composites, comprises the following steps:
Step 1: A356 aluminium alloy and the effective Aluminium Foil Package of multi-wall carbon nano-tube are wrapped up in and loads in crucible 4 according to volume fraction 50:1, fall punch 10 and compress cushion block 11, open reducing valve 1 and valve 14, pass into air pressure tank 3, pass into shielding gas by pneumatic tube 9, flow through tubing 6, finally discharged by vapor pipe 13;
Step 2: open resistance furnace 2, all melts A356 aluminium alloy in crucible 4, opens resistance furnace 12, preheating die bucket 16 and shaping die 17;
Step 3: after A356 aluminium alloy melts, open ultrasonic generator, ultrasonic amplitude bar 7 is placed in 8mm place under liquid level, ultrasonic power is 500W, ultrasonic frequency is 10kHz, meanwhile, opens magnetic stirrer 5, frequency is 2Hz, and working current is 1000A, keeps 30 minutes;
Step 4: take out ultrasonic amplitude bar 7, mouth of pot 8 is sealed, blend melt is pressed in die under the influence of air pressure, direct current is passed into coil 15, when melt is cooled to the liquid solid state temperature 575 DEG C of material, remove cushion block 12 and cushion block 18, punch 10 is descending, utilize high extrusion ratio to extrude, aligned carbon nanotube can be prepared and strengthen A356 aluminium alloy aluminum matrix composite clavate product.
Embodiment of the method 3: a kind of method preparing aligned carbon nanotube enhancing Cu-base composites, comprises the following steps:
Step 1: copper and the effective Aluminium Foil Package of single are wrapped up in and loads in crucible 4 according to volume fraction 200:1, fall punch 10 and compress cushion block 11, open reducing valve 1 and valve 14, pass into air pressure tank 3, pass into shielding gas by pneumatic tube 9, flow through tubing 6, finally discharged by vapor pipe 13;
Step 2: open resistance furnace 2, all melts A356 aluminium alloy in crucible 4, opens resistance furnace 12, preheating die bucket 16 and shaping die 17;
Step 3: after copper melts, open ultrasonic generator, ultrasonic amplitude bar 7 is placed in 5mm place under liquid level, ultrasonic power is 2000W, ultrasonic frequency is 100kHz, meanwhile, opens magnetic stirrer 5, frequency is 50Hz, and working current is 10A, keeps 25 minutes;
Step 4: take out ultrasonic amplitude bar 7, mouth of pot 8 is sealed, blend melt is pressed in die under the influence of air pressure, direct current is passed into coil 15, when melt is cooled to the liquid solid state temperature 1050 DEG C of material, remove cushion block 12 and cushion block 18, punch 10 is descending, utilize high extrusion ratio to extrude, aligned carbon nanotube can be prepared and strengthen Cu-base composites clavate product.

Claims (1)

1. one kind utilizes aligned carbon nanotube enhancing device for MMCs to prepare the method that aligned carbon nanotube strengthens metal-base composites, it is characterized in that: preparation facilities comprises reducing valve (1), first resistance furnace (2), air pressure tank (3), crucible (4), magnetic stirrer (5), tubing (6), ultrasonic amplitude bar (7), pneumatic tube (9), punch (10), upper cushion block (11), second resistance furnace (12), vapor pipe (13), valve (14), coil (15), die bucket (16), shaping die (17) and lower cushion block (18), the bottom of crucible (4) is provided with magnetic stirrer (5), ultrasonic amplitude bar (7) is equipped with at mouth of pot (8), crucible (4) is communicated with air pressure tank (3) by the pneumatic tube (9) being provided with reducing valve (1), and be communicated with die bucket (16) by tubing (6), be exhausted by the vapor pipe (13) being provided with valve (14), the first resistance furnace (2) placed outward respectively by crucible (4) and die bucket (16) and the second resistance furnace (12) heats, coil (15) is placed outward at die bucket (16) the second resistance furnace (12) outward, punch (10) and upper cushion block (11) are used for sealing die bucket (16) top, shaping die (17) and lower cushion block (18) are used for sealing die bucket (16) bottom, preparation method comprises the following steps:
Step one, raw metal and carbon nanotube aluminium foil parcel is loaded in crucible (4), fall cushion block (11) in punch (10) compression, open reducing valve (1) and valve (14), crucible (4) is communicated with air pressure tank (3), shielding gas is passed into by pneumatic tube (9), shielding gas flows through tubing (6), is finally discharged by vapor pipe (13);
Step 2, open the first resistance furnace (2), interior for crucible (4) raw metal is melted, opens the second resistance furnace (12), preheating die bucket (16) and shaping die (17);
Step 3, until raw metal melt after, open ultrasonic generator, ultrasonic amplitude bar (7) is placed in 5 ~ 10mm place under liquid level, ultrasonic power is 500 ~ 2000W, and ultrasonic frequency is 10 ~ 100kHz, meanwhile, open magnetic stirrer (5), frequency is 2Hz ~ 50Hz, and working current is 10A ~ 1000A, keeps 20-30 minute;
Step 4, taking-up ultrasonic amplitude bar (7), mouth of pot (8) is sealed, blend melt is pressed in die bucket (16) under the influence of air pressure, direct current is passed into coil (15), when melt is cooled to the liquid solid state temperature of material, remove upper cushion block (11) and lower cushion block (18), punch (10) descending extruding, realize carbon nanotube aligning in metallic matrix, obtain aligned carbon nanotube and strengthen metal-base composites.
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