CN109128174A - A kind of preparation method based on fast foaming method synthesizing carbon nanotubes enhancing foamed aluminium composite material - Google Patents

A kind of preparation method based on fast foaming method synthesizing carbon nanotubes enhancing foamed aluminium composite material Download PDF

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Publication number
CN109128174A
CN109128174A CN201811010019.9A CN201811010019A CN109128174A CN 109128174 A CN109128174 A CN 109128174A CN 201811010019 A CN201811010019 A CN 201811010019A CN 109128174 A CN109128174 A CN 109128174A
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powder
preparation
foaming
foamed aluminium
cnt
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赵乃勤
马有草
杨旭东
许佳丽
沙军威
何春年
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Tianjin University
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Tianjin University
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    • 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
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B22F3/1125—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers involving a foaming process
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • 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
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B22F3/1134—Inorganic fillers
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • 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
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C22C2026/002—Carbon nanotubes

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Catalysts (AREA)
  • Powder Metallurgy (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention relates to a kind of preparation methods based on fast foaming method synthesizing carbon nanotubes enhancing foamed aluminium composite material, including the following steps: 1) prepared by catalyst precursor: weighing pure aluminium powder and Co (NO according to the proportion that quality proportioning is 18-22:13)2·6H2O, and appropriate ethanol solution is incorporated, drying obtains precursor powder；2) preparation of CNT/Al composite powder；3) preparation of foaming presoma: by the Si powder and 0.3wt.%TiH of aforementioned obtained CNT/Al composite powder and 7wt.%2Powder mixed in three-dimensional material mixer 0.5-3h obtain uniform mixed-powder using cold press the pressure maintaining under 450MPa pressure obtain foaming presoma；4) preparation of foamed aluminium.

Description

A kind of system based on fast foaming method synthesizing carbon nanotubes enhancing foamed aluminium composite material Preparation Method
Technical field
The invention belongs to field of compound material, and in particular to a kind of application flush sintering foaming preparation carbon nanotube Enhance the research of foamed aluminium composite material.
Background technique
Foamed aluminium material as a kind of typical structure-function integration material, due to lightweight, specific strength it is high and The advantages that performances such as energy-absorbing is shockproof, damping, acoustical and thermal, electromagnetic shielding, it is widely used in aerospace, auto industry etc. Field.Document show the performance of foamed aluminium and its pore structure have it is very big be associated with, including pore size, the pore size distribution uniformity with And porosity etc..Therefore, in order to widen the application field and range of foamed aluminium, some ceramic phases introduce foam as reinforced phase Improve pore structure in aluminum substrate and promotes its performance.Although the performance of foamed aluminium achieves a degree of promotion, material Material has biggish brittleness.Therefore, it finds a kind of suitable reinforced phase and is able to maintain preferable toughness while improving intensity It is critical issue urgently to be resolved.Carbon nanotube is considered as system due to having the advantages such as density is low, intensity and modulus is high The ideal reinforced phase of standby high-performance metal based composites.Therefore, carbon nanotube is introduced into foamed aluminium matrix and is expected to realize bubble The further expansion of foam aluminium application.But the biggish draw ratio of carbon nanotube will lead to serious agglomeration, be unfavorable in base Dispersion in body.Therefore, realize carbon nanotube in the base effectively disperse and obtain Uniform pore structure be worth further investigation With the project of discussion.
Developing stage is in about the document of carbon nanotube enhancing foamed aluminium radical composite material preparation and research at present. There are three types of current main preparation methods: one is the method combined using colloid technique and prior powder metallurgy, being for second Using the method for flux foaming, the third is using addition pore-creating agent method of the urea as pore creating material.It can be at by these Function, which prepares carbon nanotube, enhances foamed aluminium radical composite material, but still has some problems.On the one hand, preparation process is more multiple Miscellaneous, efficiency is lower；On the other hand, external carbon pipe is inclined to stronger reunion, and the methods of mechanical stirring can not achieve well Dispersion.Therefore, find a kind of high-efficient and carbon nanotube can evenly dispersed method in the base be necessary.
Flush sintering foaming is a kind of new method for preparing foamed aluminium, and process flow is simple and cost is relatively low. But the research at present about this method is less, and is confined to some traditional reinforced phases (such as SiC etc.) and alloying element The influence of (Si, Mg etc.) to foaming process.Carbon nanotube is introduced into flush sintering foaming as reinforced phase and is expected to Realize the efficient preparation of carbon nanotube enhancing foamed aluminium radical composite material.
Summary of the invention
The present invention provides a kind of preparation of efficient and finely dispersed synthesizing carbon nanotubes enhancing foamed aluminium composite material Method.To solve the problems, such as that carbon nanotube is reunited in the base, the method that the present invention uses in-situ chemical vapor deposition, i.e., with equal The even nanometre grade cobalt particle for being dispersed in aluminium powder surface is catalyst, at 600 DEG C, using acetylene as carbon source, carries out situ catalytic growth. Carbon nanotube may be implemented by this method in the evenly dispersed of aluminium powder surface, while can also in final foamed aluminium matrix To be kept well.Meanwhile by the addition by control different content carbon pipe, the abscess of foamed aluminium can be adjusted Control.Technical solution is as follows:
A kind of preparation method based on fast foaming method synthesizing carbon nanotubes enhancing foamed aluminium composite material, including following step It is rapid:
1) prepared by catalyst precursor: weighing pure aluminium powder and Co (NO according to the proportion that quality proportioning is 18-22:13)2· 6H2O, and appropriate ethanol solution is incorporated, first stirring in water bath heats ultrasound under conditions of 60-80 DEG C again, after 2-4h Alcohol is evaporated volatilization, and rear drying obtains precursor powder.
2) preparation of CNT/Al composite powder: 10-30g precursor powder is put into the corundum Noah's ark for being placed in tube furnace, It is heated to 250 DEG C under an argon atmosphere, is then heated to 450 DEG C in a hydrogen atmosphere, reductase 12-4h, later under the conditions of argon gas 600 DEG C of progress chemical vapor depositions are heated to, the atmospheric condition of chemical vapor deposition is that acetylene and argon gas are divided into for 10-30ml/ Min and 150-250ml/min obtains CNT/Al composite powder；
3) preparation of foaming presoma: by the Si powder and 0.3wt.% of aforementioned obtained CNT/Al composite powder and 7wt.% TiH2Powder mixes 0.5-3h in three-dimensional material mixer and obtains uniform mixed-powder to be protected under 450MPa pressure using cold press Pressure obtains foaming presoma；
4) preparation of foamed aluminium: foaming presoma is preheated to 740 DEG C in foaming furnace, is then placed in foaming presoma Heat preservation a period of time takes out in mold, carries out quick water cooling to mold, obtains carbon nanotube enhancing foamed aluminium composite material.
In conclusion core of the invention is to realize it in matrix using in-situ chemical vapor deposition synthesizing carbon nanotubes In it is evenly dispersed, using fast foaming method realize composite material efficient preparation, and by control carbon pipe content control foam The hole pattern of aluminium sample, reaches the controllable preparation of Different Pore Structures foamed aluminium sample.Compared with prior art, of the invention excellent Point is:
(1) present invention realizes carbon nanotube in aluminium powder surface and foamed aluminium matrix by in-situ chemical vapor deposition method It is evenly dispersed.
(2) Preparation equipment of the present invention is simple, simple process, using fast foaming technique, after foam presoma and preheating It mold direct contact heat transfer and foams in confinement space, preparation efficiency is significantly improved.
(3) present invention uses fast foaming, and the short structural intergrity to ensure that carbon pipe of foamed time is allowed in foam Higher quality is still maintained in aluminum substrate.
(4) present invention realizes the controllableization preparation of Different Pore Structures by the introducing of carbon nanotube.
Detailed description of the invention
Fig. 1 is that evenly dispersed carbon nanotube is schemed in the SEM of foamed aluminium hole wall surface.
Fig. 2 is the Raman comparison diagram of composite powder and compound foamed aluminum sample after foaming after chemical vapor deposition.
Fig. 3 is the compound foamed aluminum of the obtained Different Pore Structures of different carbon pipe contents prepared by the present invention.
Specific embodiment
The technology of the present invention route is as follows:
1) prepared by catalyst precursor: by the Co (NO of 19.9g pure aluminium powder and 0.4949g3)2·6H2O is 150-250ml's Ultrasound 30-60min in ethanol solution, then stirring in water bath heats under conditions of 60-80 DEG C again, and alcohol steams after 2-4h Then dry volatilization dries 8-16h in an oven and obtains precursor powder；
2) preparation of CNT/Al composite powder: 10-30g precursor powder is put into the corundum Noah's ark for being placed in tube furnace, 250 DEG C are heated under argon gas (120-400ml/min) atmosphere, is then heated to 450 under hydrogen (150-250ml/min) atmosphere DEG C, reductase 12-4h is heated to 600 DEG C of progress chemical vapor deposition 10-120min under the conditions of argon gas later, and atmospheric condition is second Alkynes and argon gas (10-30ml/min, 150-250ml/min), obtain CNT/Al composite powder；
3) preparation of foaming presoma: by the Si powder and 0.3wt.% of aforementioned obtained CNT/Al composite powder and 7wt.% TiH2Powder mixes 0.5-3h in three-dimensional material mixer and obtains uniform mixed-powder, then weighs 24g powder and uses cold press Pressure maintaining 5min obtains 38 × 8mm of Φ under 450MPa pressure3Cylindrical body foaming presoma；
4) preparation of foamed aluminium: preheating 20-60min to 740 DEG C for the cylinder mold of Φ 38 in foaming furnace, then will Foaming presoma, which is placed in mold, keeps the temperature 90s taking-up, carries out quick water cooling to mold, obtains nearly columned sample, this process In realize and be rapidly heated and cool down.Sample after cooling carries out wire cutting to carry out other tests as needed later.
Below with reference to examples illustrate the present invention.
Example 1
By the Si powder and 0.3wt.%TiH of pure aluminium powder and 7wt.%2Powder mixes 2h in three-dimensional material mixer and obtains uniformly Mixed-powder, then weighing 24g powder, the pressure maintaining 5min under 450MPa pressure obtains 38 × 8mm of Φ using cold press3Circle The foaming presoma of cylinder；The cylinder mold of Φ 38 is preheated 40min to 740 DEG C in foaming furnace, then will foam forerunner Body, which is placed in mold, keeps the temperature 90s taking-up, carries out quick water cooling to mold, obtains nearly columned sample, carry out wire cutting later Obtain 20 × 20 × 20mm3Sample, such as Fig. 3 a and 3e, average pore size 2.29mm, porosity 78.1%.
Example 2
By the Co (NO of 19.9g pure aluminium powder and 0.4949g3)2·6H2O is ultrasonic in the ethanol solution of 150ml 30min, then stirring in water bath heats under conditions of 60 DEG C again, and alcohol is evaporated volatilization after 4h, then dry 8h in an oven Obtain precursor powder；20g precursor powder is put into the corundum Noah's ark for being placed in tube furnace, argon gas (300ml/min) atmosphere Under be heated to 250 DEG C, then 450 DEG C, reductase 12 .5h are heated under hydrogen (250ml/min) atmosphere, later in argon gas condition Under be heated to 600 DEG C of progress chemical vapor deposition 10min, atmospheric condition is acetylene and argon gas (20ml/min, 240ml/min), Obtain 0.5wt.%CNT/Al composite powder；By the Si powder and 0.3wt.% of aforementioned obtained CNT/Al composite powder and 7wt.% TiH2Powder mixes 1h in three-dimensional material mixer and obtains uniform mixed-powder, then weighs 24g powder and is existed using cold press Pressure maintaining 5min obtains 38 × 8mm of Φ under 450MPa pressure3Cylindrical body foaming presoma；The cylinder mold of Φ 38 is being sent out It steeps and preheats 20min to 740 DEG C in furnace, then foaming presoma is placed in mold and keeps the temperature 90s taking-up, quick water is carried out to mold It is cold, nearly columned sample is obtained, wire cutting is carried out later and obtains 20 × 20 × 20mm3Sample, such as Fig. 3 b and 3f, average hole Diameter 2.19mm, porosity 76.5%.
Example 3
By the Co (NO of 19.9g pure aluminium powder and 0.4949g3)2·6H2O is ultrasonic in the ethanol solution of 200ml 40min, then stirring in water bath heats under conditions of 70 DEG C again, and alcohol is evaporated volatilization after 3h, then dry 10h in an oven Obtain precursor powder；20g precursor powder is put into the corundum Noah's ark for being placed in tube furnace, argon gas (250ml/min) atmosphere Under be heated to 250 DEG C, be then heated to 450 DEG C under hydrogen (200ml/min) atmosphere, reductase 12 h, later under the conditions of argon gas 600 DEG C of progress chemical vapor deposition 20min are heated to, atmospheric condition is acetylene and argon gas (20ml/min, 240ml/min), is obtained To 1.0wt.%CNT/Al composite powder；By the Si powder and 0.3wt.% of aforementioned obtained CNT/Al composite powder and 7wt.% TiH2Powder mixes 0.5h in three-dimensional material mixer and obtains uniform mixed-powder, then weighs 24g powder and is existed using cold press Pressure maintaining 5min obtains 38 × 8mm of Φ under 450MPa pressure3Cylindrical body foaming presoma；The cylinder mold of Φ 38 is being sent out It steeps and preheats 35min to 740 DEG C in furnace, then foaming presoma is placed in mold and keeps the temperature 90s taking-up, quick water is carried out to mold It is cold, nearly columned sample is obtained, wire cutting is carried out later and obtains 20 × 20 × 20mm3Sample, such as Fig. 3 c and 3g, average hole Diameter 2.13mm, porosity 75.9%.
Example 4
By the Co (NO of 19.9g pure aluminium powder and 0.4949g3)2·6H2O is ultrasonic in the ethanol solution of 175ml 60min, then stirring in water bath heats under conditions of 80 DEG C again, and alcohol is evaporated volatilization after 2h, then dry 12h in an oven Obtain precursor powder；20g precursor powder is put into the corundum Noah's ark for being placed in tube furnace, argon gas (280ml/min) atmosphere Under be heated to 250 DEG C, be then heated to 450 DEG C under hydrogen (180ml/min) atmosphere, 3h restored, later under the conditions of argon gas 600 DEG C of progress chemical vapor deposition 30min are heated to, atmospheric condition is acetylene and argon gas (20ml/min, 240ml/min), is obtained To 1.5wt.%CNT/Al composite powder；By the Si powder and 0.3wt.% of aforementioned obtained CNT/Al composite powder and 7wt.% TiH2Powder mixes 3h in three-dimensional material mixer and obtains uniform mixed-powder, then weighs 24g powder and is existed using cold press Pressure maintaining 5min obtains 38 × 8mm of Φ under 450MPa pressure3Cylindrical body foaming presoma；The cylinder mold of Φ 38 is being sent out It steeps and preheats 50min to 740 DEG C in furnace, then foaming presoma is placed in mold and keeps the temperature 90s taking-up, quick water is carried out to mold It is cold, nearly columned sample is obtained, wire cutting is carried out later and obtains 20 × 20 × 20mm3Sample, such as Fig. 3 d and 3h, average hole Diameter 2.01mm, porosity 74.2%.

Claims (1)

1. a kind of preparation method based on fast foaming method synthesizing carbon nanotubes enhancing foamed aluminium composite material, including following step It is rapid:
1) prepared by catalyst precursor: weighing pure aluminium powder and Co (NO according to the proportion that quality proportioning is 18-22:13)2·6H2O, And appropriate ethanol solution is incorporated, first stirring in water bath heats ultrasound under conditions of 60-80 DEG C again, and alcohol steams after 2-4h Dry volatilization, rear drying obtain precursor powder.
2) preparation of CNT/Al composite powder: 10-30g precursor powder is put into the corundum Noah's ark for being placed in tube furnace, in argon It is heated to 250 DEG C under gas atmosphere, is then heated to 450 DEG C in a hydrogen atmosphere, reductase 12-4h is heated under the conditions of argon gas later To 600 DEG C of progress chemical vapor depositions, the atmospheric condition of chemical vapor deposition is acetylene and argon gas is divided into for 10-30ml/min and 150-250ml/min obtains CNT/Al composite powder；
3) preparation of foaming presoma: by the Si powder and 0.3wt.%TiH of aforementioned obtained CNT/Al composite powder and 7wt.%2 Powder mixes 0.5-3h in three-dimensional material mixer and obtains uniform mixed-powder the pressure maintaining under 450MPa pressure obtains using cold press To foaming presoma；
4) preparation of foamed aluminium: foaming presoma is preheated to 740 DEG C in foaming furnace, foaming presoma is then placed in mold Middle heat preservation a period of time takes out, and carries out quick water cooling to mold, obtains carbon nanotube enhancing foamed aluminium composite material.
CN201811010019.9A 2018-08-31 2018-08-31 A kind of preparation method based on fast foaming method synthesizing carbon nanotubes enhancing foamed aluminium composite material Pending CN109128174A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114702325A (en) * 2022-02-11 2022-07-05 惠州学院 Method for uniformly mixing silicon-based nano phase with large length-diameter ratio in ceramic powder

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103352134A (en) * 2013-06-27 2013-10-16 天长市京发铝业有限公司 Melt-foaming preparation method of foamed aluminum material
CN104745976A (en) * 2015-03-27 2015-07-01 中国民航大学 Preparation method of carbon-nanotube-reinforced foamed aluminum-base composite material
CN104745853A (en) * 2015-04-23 2015-07-01 苏州第一元素纳米技术有限公司 Preparation method of foamed aluminum/ nano carbon composite material
CN106984818A (en) * 2017-02-28 2017-07-28 东莞市佳乾新材料科技有限公司 A kind of nanometer foam aluminium composite sandwich panel with gradient interface and preparation method thereof
CN107675015A (en) * 2017-10-11 2018-02-09 中国民航大学 A kind of closed pore CNTs/Al Si composite foam materials and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103352134A (en) * 2013-06-27 2013-10-16 天长市京发铝业有限公司 Melt-foaming preparation method of foamed aluminum material
CN104745976A (en) * 2015-03-27 2015-07-01 中国民航大学 Preparation method of carbon-nanotube-reinforced foamed aluminum-base composite material
CN104745853A (en) * 2015-04-23 2015-07-01 苏州第一元素纳米技术有限公司 Preparation method of foamed aluminum/ nano carbon composite material
CN106984818A (en) * 2017-02-28 2017-07-28 东莞市佳乾新材料科技有限公司 A kind of nanometer foam aluminium composite sandwich panel with gradient interface and preparation method thereof
CN107675015A (en) * 2017-10-11 2018-02-09 中国民航大学 A kind of closed pore CNTs/Al Si composite foam materials and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114702325A (en) * 2022-02-11 2022-07-05 惠州学院 Method for uniformly mixing silicon-based nano phase with large length-diameter ratio in ceramic powder

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Application publication date: 20190104