CN109175374A - The preparation method of the foamed aluminium filling aluminium-alloy pipe composite construction of carbon nanotube enhancing - Google Patents
The preparation method of the foamed aluminium filling aluminium-alloy pipe composite construction of carbon nanotube enhancing Download PDFInfo
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- CN109175374A CN109175374A CN201810944760.6A CN201810944760A CN109175374A CN 109175374 A CN109175374 A CN 109175374A CN 201810944760 A CN201810944760 A CN 201810944760A CN 109175374 A CN109175374 A CN 109175374A
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- aluminium
- carbon nanotube
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- alloy pipe
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Classifications
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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
-
- 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
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- 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
Abstract
The present invention relates to a kind of carbon nanotube enhancing foamed aluminium filling aluminium-alloy pipe composite construction preparation method, realized by following steps: prepare aluminium powder surface uniform load the composite powder of carbon nanotube；Mechanical ball mill；Composite powder after ball milling is uniformly mixed with urea, cold moudling；Sample after cold pressing removes urea in 60-80 DEG C of at a temperature of water-bath 6-8h, and sample is placed in baking oven after water-bath and is dried；Sample after drying is placed in tube furnace, is sintered 2-4h at being warming up to 650 DEG C under the argon gas protection of 200-300ml/min flow with the rate of 5 DEG C/min, is cooled to room temperature after the completion of sintering with the furnace；Obtain the foamed aluminium filling aluminium-alloy pipe composite construction of carbon nanotube enhancing.
Description
Technical field
The invention belongs to foamed aluminium filled composite structure preparation technical field, it is related to making with the carbon nanotube of growth in situ
For reinforced phase, and metal tube is filled using composite foam material as core material and realizes collaboration enhancing, so that high intensity is realized, it is high
The preparation of the interstitital texture of energy-absorbing.
Background technique
Representative of the foamed aluminium as structure-function integration material, since with matrix element rich reserves, density is low, hinders
The excellent performances such as damping properties are good, energy absorption ability is strong are gradually applied in recent years in every field such as aerospace, rail traffics.But
Foamed aluminium can bear that load is small when being used alone, and the defect that easy unstability is collapsed is limited by very large its application.Thin-walled
The bearing capacity of pipe structure axial direction is stablized, and it is traditional energy-absorbing vibration-absorptive material that operation mileage rate is long, but its there is also non axial carryings
The problems such as ability is poor, and failure procedure is difficult to control.By the interstitital texture of foamed aluminium and the compound preparation of thin-wall metal pipe, make up
The disadvantage of foamed aluminium and metal tube respectively both has independent bearing ability, high but also with stability, can be in extreme environments
Outstanding advantages of military service, therefore the common concern by researcher.It is existing experiments have shown that filled and process aluminium helps to promote at present
Also indicate that metal tube according to more stably and controllable mode deformation, but simultaneously, only the intensity of foamed aluminium and metal pipe-wall
Intensity is just able to achieve when realizing good matching obtains higher bearing capacity and better energy-absorbing effect.
Carbon nanotube (CNTs) is multiple due to being widely regarded as Metal Substrate with excellent properties such as low-density, high specific strengths
The ideal reinforced phase of condensation material.Composite material especially is prepared using CNTs as reinforced phase, traditional material can be overcome to answer
With some limitations.However since CNTs has biggish draw ratio, causes CNTs and easily reunites in aluminum substrate, it is difficult to
It realizes evenly dispersed.Currently used dispersing method can cause serious destruction to the structure of CNTs.And use in-situ chemical
Vapour deposition process has synthesized CNTs on aluminium powder surface, then prepares CNTs enhancing by ball milling in short-term and the method for dosing pore creating material
The method of compound foamed aluminum had not only solved the problems, such as the additive amount that is evenly dispersed, improving carbon pipe of CNTs, but also can make metallic matrix
Good interface cohesion is formed between CNTs.
In conclusion use the CNTs/Al composite powder of vapour deposition process preparation in situ combine dose pore creating material method can be with
Realize the preparation of high-intensitive carbon nanotube enhancing compound foamed aluminum.It is refilled by the way that composite foam surface is slightly polished into interior
The close knot of foam and metal pipe-wall can be realized in diameter and the consistent metal tube of foam diameter in a kind of relatively simple mode
It closes.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation processes, and simple, foam parameters accurately control, product damping energy-absorbing is imitated
The preparation method of the foamed aluminium filling metal tube composite construction of the good carbon nanotube enhancing of fruit.The technical solution of the present invention is as follows:
A kind of preparation method of the foamed aluminium filling aluminium-alloy pipe composite construction of carbon nanotube enhancing, passes through following steps reality
It is existing:
(1) by aluminium powder and cabaltous nitrate hexahydrate according to the mass ratio of 160-40:1 be added to that quality is aluminium powder 5-10 times
In dehydrated alcohol, accelerates the dissolution of cobalt nitrate using ultrasound, be stirred continuously until that ethyl alcohol is waved in 60 DEG C of heating water bath later
It distributes complete.Obtained mixture is placed in again in 80 DEG C of baking oven and is dried 6 hours or more, the complete powder of obtained drying is set
In tube furnace, it is warming up to 250 DEG C under the protection of argon gas, switches to flow and is the hydrogen of 200-300ml/min, and exist respectively
1 hour is kept the temperature at 250 DEG C and 450 DEG C respectively；It is then turned off hydrogen, 600 DEG C are warming up under the protection of argon gas, and according to acetylene
The mixed gas of the two is passed through for the ratio of 1:12 with argon gas, is reacted 15-60m minutes at 600 DEG C, finally closes gaseous mixture,
Be cooled to room temperature under the protection of argon gas, obtain aluminium powder surface uniform load the composite powder of carbon nanotube；
(2) composite powder for obtaining step (1) carries out mechanical ball mill, and ratio of grinding media to material is that 10-15:1 rotational speed of ball-mill is 300-
450rpm, ball milling 60-120min；
(3) composite powder after ball milling is uniformly mixed with the urea that the diameter of its quality 70%-200% is 1-3mm, it will
Mixture is placed in cold stamping die, and pressure maintaining 3-5min realizes cold moudling at 400-500MPa；
(4) sample after being cold-pressed removes urea in 60-80 DEG C of at a temperature of water-bath 6-8h, and sample is placed in baking oven after water-bath
Middle drying；
(5) sample after drying is placed in tube furnace, with 5 DEG C/min under the argon gas protection of 200-300ml/min flow
Rate be warming up at 650 DEG C and be sintered 2-4h, cool to room temperature after the completion of sintering with the furnace；
(6) it is inserted in thin-walled hollow aluminium-alloy pipe after sintered specimen surface slightly being polished, obtains carbon nanotube increasing
Strong foamed aluminium fills aluminium-alloy pipe composite construction.
Foamed aluminium filling aluminium-alloy pipe composite construction of carbon nanotube enhancing of the invention and preparation method thereof has following
The utility model has the advantages that
(1) present invention, which uses, carries out the composite foam aluminium surface that carbon nanometer enhances directly to insert aluminium alloy after slightly polishing
Method in pipe realizes filling, greatly reduces the gap between filling core material and metal pipe-wall, make metal tube and foam it
Between realize good load transmission, enhance damping energy-absorbing effect.
(2) it in the preparation method for the aperture CNTs/Al composite foam that the present invention includes, prepared by in-situ chemical vapor deposition
CNTs/Al composite powder carries out mechanical ball mill in short-term, makes in CTS insertion Al matrix, to make to have between aluminum particle more preferable
Binding force.To play with better reinforcing effect.
(3) foamed aluminium material is aperture in the foamed aluminium filling aluminium-alloy pipe composite construction of carbon nanotube of the invention enhancing
Structure, distribution of cells is uniform, and abscess-size is uniform, and aperture is controllable between 1-3 mm.Its compressive stress strain curve exists
The apparent higher platform area of stress value, so that composite foam has higher energy-absorbing damping effect.
(4) the preparation method use of this technique doses pore creating material method and prepares composite foam, and the hole for foam may be implemented
Gap rate, pore size and aperture uniform level accurately control, and CNTS/A composite foam linear zone of the invention is smooth, platform area
Stress is reachable~30MPa, substantially increase its energy absorption performance.And the energy absorption curve of interstitital texture is much higher than foamed material and metal
The sum of energy absorption curve of pipe.
Detailed description of the invention
Illustrate the embodiment of the present invention or technical solution in the prior art in order to clearer, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it is clear that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Other attached drawings are obtained according to these attached drawings.
Fig. 1 is the main view that the foamed aluminium that carbon nanotube of the invention enhances fills aluminium-alloy pipe composite construction；
Fig. 2 is the intermediate cross-section side view that the foamed aluminium that carbon nanotube of the invention enhances fills aluminium-alloy pipe composite construction
Figure；
Fig. 3 is the load-deformation curve and compound vacuole of composite foam interstitital texture obtained made from the embodiment of the present invention 1
The comparison diagram of the load-deformation curve of foam and metal tube adduction (composite foam porosity is 60%).
Fig. 4 is the stress-strain of composite foam interstitital texture and fine aluminium foam interstitital texture made from the embodiment of the present invention 1
Curve comparison figure (composite foam and fine aluminium foam porosities are 60%)；
Fig. 5 be interstitital texture made from the embodiment of the present invention 1 energy absorption curve and foam and metal tube energy absorption curve it
With comparison diagram (composite foam porosity is 60%).
Specific embodiment
Below in conjunction with the attached drawing in the present invention, technical solution in the embodiment of the present invention carry out it is clear, completely retouch
It states.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, those skilled in the art's all other reality obtained without making creative work
Example is applied, protection scope of the present invention is belonged to.
Embodiment 1
The preparation method of aperture CNTs/Al composite foam is the following steps are included: aluminium powder and six are hydrated by (1) in the present embodiment
Cobalt nitrate is added in 7 times of the dehydrated alcohol that quality is aluminium powder according to the mass ratio of 40:1.Accelerate cobalt nitrate using ultrasound
Dissolution is stirred continuously until that ethyl alcohol volatilization is complete in 60 DEG C of heating water bath later.Obtained mixture is placed in 80 DEG C again
Baking oven in dry 8 hours.The complete powder of obtained drying is placed in tube furnace, is warming up to 250 under the protection of argon gas
DEG C, it switches to flow and is the hydrogen of 200ml/min, and keep the temperature 1 hour respectively at 250 DEG C and 450 DEG C respectively.It is then turned off hydrogen
Gas is warming up to 600 DEG C under the protection of argon gas, and is that the ratio of 1:12 is passed through the mixed gas of the two according to acetylene and argon gas,
It is reacted 30m minutes at 600 DEG C, finally closes gaseous mixture, be cooled to room temperature under the protection of argon gas, it is uniform to obtain aluminium powder surface
Load the composite powder of carbon nanotube；
(2) composite powder for obtaining step (1) carries out mechanical ball mill, and ratio of grinding media to material is that 10:1 rotational speed of ball-mill is 400rpm,
Ball milling 90min；
(3) composite powder after ball milling is uniformly mixed with the urea that the diameter of its quality 75% is 2.5mm.By mixture
It is placed in cold stamping die, pressure maintaining 5min realizes cold moudling at 500MPa (composite foam porosity obtained is 60%)；
(4) sample after being cold-pressed removes urea in 80 DEG C of at a temperature of water-bath 6h, and sample is placed in baking oven after water-bath and is dried
It is dry；
(5) sample after drying is placed in tube furnace, with the speed of 5 DEG C/min under the argon gas protection of 200ml/min flow
Rate, which is warming up at 650 DEG C, is sintered 3h, cools to room temperature after the completion of sintering with the furnace；
(6) it is inserted in thin-walled hollow aluminium-alloy pipe after sintered specimen surface slightly being polished, obtains carbon nanotube increasing
Strong foamed aluminium fills aluminium-alloy pipe composite construction.The pipe wall internal diameters of thin-wall metal pipe and the diameter dimension of composite foam are consistent,
Need to be by the way that foam be inserted in metal tube again after slightly polishing composite foam surface, gap as far as possible between holding foam and tube wall
It is minimum.
The component is cylindrical-shaped structure, and outer wall is 6061 aluminum alloy thin walled pipes, and internal filled core is that the carbon of growth in situ is received
The foamed aluminium core material of mitron enhancing.The foamed aluminium is open-celled structure.This kind of composite filled structure, it is independent to compensate for foamed aluminium
It can bear that load is small when use, the defect and the non axial bearing capacity of metal tube that easy unstability is collapsed are poor, and failure procedure is difficult to control,
Lateral energy-absorbing effect is nothing like the problems such as longitudinal.The existing independent bearing ability of this kind of composite construction, but also with stability
High, outstanding advantages of being on active service in extreme environments.The composite construction can absorb more energy in deformation process, real
Existing good damping energy-absorbing, the shock proof effect of crashworthiness.The present invention has extremely huge application potential in auto manufacturing, can
In practical applications as the shock proof protection structure of energy-absorbing damping.
Embodiment 2
The preparation method of aperture CNTs/Al composite foam is the following steps are included: aluminium powder and six are hydrated by (1) in the present embodiment
Cobalt nitrate is added in 10 times of the dehydrated alcohol that quality is aluminium powder according to the mass ratio of 80:1.Accelerate cobalt nitrate using ultrasound
Dissolution is stirred continuously until that ethyl alcohol volatilization is complete in 60 DEG C of heating water bath later.Obtained mixture is placed in 80 DEG C again
Baking oven in dry 8 hours.By in the complete powder tube furnace of obtained drying, it is warming up to 250 DEG C under the protection of argon gas, cuts
It shifts to flow and is the hydrogen of 250ml/min, and keep the temperature 1 hour respectively at 250 DEG C and 450 DEG C respectively.It is then turned off hydrogen,
It is warming up to 600 DEG C under the protection of argon gas, and is that the ratio of 1:12 is passed through the mixed gas of the two according to acetylene and argon gas, 600
It is reacted 60m minutes at DEG C, finally closes gaseous mixture, be cooled to room temperature under the protection of argon gas, obtain aluminium powder surface uniform load
The composite powder of carbon nanotube；
(2) composite powder for obtaining step (1) carries out mechanical ball mill, and ratio of grinding media to material is that 15:1 rotational speed of ball-mill is 350rpm,
Ball milling 90min；
(3) composite powder after ball milling is uniformly mixed with the urea that the diameter of its quality 115% is 2mm.By mixture
It is placed in cold stamping die, pressure maintaining 3min realizes cold moudling at 500MPa (composite foam porosity obtained is 70%)；
(4) sample after being cold-pressed removes urea in 80 DEG C of at a temperature of water-bath 6h, and sample is placed in baking oven after water-bath and is dried
It is dry；
(5) sample after drying is placed in tube furnace, with the speed of 5 DEG C/min under the argon gas protection of 250ml/min flow
Rate, which is warming up at 650 DEG C, is sintered 3h, cools to room temperature after the completion of sintering with the furnace；
(6) it is inserted in thin-walled hollow aluminium-alloy pipe after sintered specimen surface slightly being polished, obtains carbon nanotube increasing
Strong foamed aluminium fills aluminium-alloy pipe composite construction.
Embodiment 3
The preparation method of aperture CNTs/Al composite foam is the following steps are included: aluminium powder and six are hydrated by (1) in the present embodiment
Cobalt nitrate is added in 8 times of the dehydrated alcohol that quality is aluminium powder according to the mass ratio of 120:1.Accelerate cobalt nitrate using ultrasound
Dissolution is stirred continuously until that ethyl alcohol volatilization is complete in 60 DEG C of heating water bath later.Obtained mixture is placed in 80 DEG C again
Baking oven in dry 8 hours.The complete powder of obtained drying is placed in tube furnace, is warming up to 250 under the protection of argon gas
DEG C, it switches to flow and is the hydrogen of 240ml/min, and keep the temperature 1 hour respectively at 250 DEG C and 450 DEG C respectively.It is then turned off hydrogen
Gas is warming up to 600 DEG C under the protection of argon gas, and is that the ratio of 1:12 is passed through the mixed gas of the two according to acetylene and argon gas,
It is reacted 60m minutes at 600 DEG C, finally closes gaseous mixture, be cooled to room temperature under the protection of argon gas, it is uniform to obtain aluminium powder surface
Load the composite powder of carbon nanotube；
(2) composite powder for obtaining step (1) carries out mechanical ball mill, and ratio of grinding media to material is that 10:1 rotational speed of ball-mill is 400rpm,
Ball milling 60min；
(3) composite powder after ball milling is uniformly mixed with the urea that the diameter of its quality 75% is 2.5mm, the matter of urea
Amount is the 40%-79% of mixture quality.Mixture is placed in cold stamping die, pressure maintaining 5min realization is cold-pressed at 500MPa
Type (composite foam porosity obtained is 60%)；
(4) sample after being cold-pressed removes urea in 60 DEG C of at a temperature of water-bath 8h, and sample is placed in baking oven after water-bath and is dried
It is dry；
(5) sample after drying is placed in tube furnace, with the speed of 5 DEG C/min under the argon gas protection of 240ml/min flow
Rate, which is warming up at 650 DEG C, is sintered 2.5h, cools to room temperature after the completion of sintering with the furnace；
(6) it is inserted in thin-walled hollow aluminium-alloy pipe after sintered specimen surface slightly being polished, obtains carbon nanotube increasing
Strong foamed aluminium fills aluminium-alloy pipe composite construction.
Embodiment 4
The preparation method of aperture CNTs/Al composite foam is the following steps are included: aluminium powder and six are hydrated by (1) in the present embodiment
Cobalt nitrate is added in 10 times of the dehydrated alcohol that quality is aluminium powder according to the mass ratio of 40:1.Accelerate cobalt nitrate using ultrasound
Dissolution is stirred continuously until that ethyl alcohol volatilization is complete in 60 DEG C of heating water bath later.Obtained mixture is placed in 80 DEG C again
Baking oven in dry 8 hours.The complete powder of obtained drying is placed in tube furnace, is warming up to 250 under the protection of argon gas
DEG C, it switches to flow and is the hydrogen of 200ml/min, and keep the temperature 1 hour respectively at 250 DEG C and 450 DEG C respectively.It is then turned off hydrogen
Gas is warming up to 600 DEG C under the protection of argon gas, and is that the ratio of 1:12 is passed through the mixed gas of the two according to acetylene and argon gas,
It is reacted 15m minutes at 600 DEG C, finally closes gaseous mixture, be cooled to room temperature under the protection of argon gas, it is uniform to obtain aluminium powder surface
Load the composite powder of carbon nanotube；
(2) composite powder for obtaining step (1) carries out mechanical ball mill, and ratio of grinding media to material is that 10:1 rotational speed of ball-mill is 350rpm,
Ball milling 120min；
(3) composite powder after ball milling is uniformly mixed with the urea that the diameter of its quality 195% is 1.5mm, urea
Quality is the 40%-79% of mixture quality.Mixture is placed in cold stamping die, pressure maintaining 5min realizes cold pressing at 450MPa
Molding (composite foam porosity obtained is 80%)；
(4) sample after being cold-pressed removes urea in 80 DEG C of at a temperature of water-bath 8h, and sample is placed in baking oven after water-bath and is dried
It is dry；
(5) sample after drying is placed in tube furnace, with the speed of 5 DEG C/min under the argon gas protection of 240ml/min flow
Rate, which is warming up at 650 DEG C, is sintered 3h, cools to room temperature after the completion of sintering with the furnace；
(6) it is inserted in thin-walled hollow aluminium-alloy pipe after sintered specimen surface slightly being polished, obtains carbon nanotube increasing
Strong foamed aluminium fills aluminium-alloy pipe composite construction.
Claims (1)
1. a kind of preparation method of the foamed aluminium filling aluminium-alloy pipe composite construction of carbon nanotube enhancing, passes through following steps reality
It is existing:
(1) by aluminium powder and cabaltous nitrate hexahydrate according to the anhydrous of the mass ratio of 160-40:1 be added to that quality is aluminium powder 5-10 times
In ethyl alcohol, accelerates the dissolution of cobalt nitrate using ultrasound, be stirred continuously until that ethyl alcohol is evaporated completely in 60 DEG C of heating water bath later
Entirely.Obtained mixture is placed in again in 80 DEG C of baking oven and is dried 6 hours or more, the complete powder of obtained drying is placed in pipe
In formula furnace, it is warming up to 250 DEG C under the protection of argon gas, switches to the hydrogen that flow is 200-300ml/min, and respectively 250
DEG C and 450 DEG C at keep the temperature 1 hour respectively；Be then turned off hydrogen, be warming up to 600 DEG C under the protection of argon gas, and according to acetylene and
Argon gas is the mixed gas that the ratio of 1:12 is passed through the two, reacts 15-60m minutes at 600 DEG C, finally closes gaseous mixture,
Be cooled to room temperature under the protection of argon gas, obtain aluminium powder surface uniform load the composite powder of carbon nanotube；
(2) composite powder for obtaining step (1) carries out mechanical ball mill, and ratio of grinding media to material is that 10-15:1 rotational speed of ball-mill is 300-
450rpm, ball milling 60-120min；
(3) composite powder after ball milling is uniformly mixed with the urea that the diameter of its quality 70%-200% is 1-3mm, will be mixed
Object is placed in cold stamping die, and pressure maintaining 3-5min realizes cold moudling at 400-500MPa；
(4) sample after being cold-pressed removes urea in 60-80 DEG C of at a temperature of water-bath 6-8h, and sample is placed in baking oven after water-bath and is dried
It is dry；
(5) sample after drying is placed in tube furnace, with the speed of 5 DEG C/min under the argon gas protection of 200-300ml/min flow
Rate, which is warming up at 650 DEG C, is sintered 2-4h, cools to room temperature after the completion of sintering with the furnace；
(6) it is inserted in thin-walled hollow aluminium-alloy pipe after sintered specimen surface slightly being polished, obtains carbon nanotube enhancing
Foamed aluminium fills aluminium-alloy pipe composite construction.
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| CN109913776A (en) * | 2019-03-28 | 2019-06-21 | 中国飞机强度研究所 | A kind of fiber reinforcement Open-cell Aluminum Foam and preparation method thereof |
| CN109909504A (en) * | 2019-02-28 | 2019-06-21 | 昆明理工大学 | A kind of porous foam enhancing metallic composite and preparation method thereof |
| CN111636047A (en) * | 2020-05-29 | 2020-09-08 | 太原理工大学 | Method for preparing antibacterial alloy nano-column on surface of medical metal |
| CN113073237A (en) * | 2021-03-22 | 2021-07-06 | 中国民航大学 | Preparation method of carbon nano tube reinforced aluminum-based composite foam material for electromagnetic shielding |
| CN114054722A (en) * | 2021-11-18 | 2022-02-18 | 河北工业大学 | High-overload-resistant foamed zinc-aluminum eutectoid alloy/aluminum alloy composite material and preparation method thereof |
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| CN109909504A (en) * | 2019-02-28 | 2019-06-21 | 昆明理工大学 | A kind of porous foam enhancing metallic composite and preparation method thereof |
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Application publication date: 20190111 |