CN106555071B - In the method that aluminium powder surface in situ catalysis gaseous carbon source prepares CNT/aluminium composite material - Google Patents
In the method that aluminium powder surface in situ catalysis gaseous carbon source prepares CNT/aluminium composite material Download PDFInfo
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- CN106555071B CN106555071B CN201611088685.5A CN201611088685A CN106555071B CN 106555071 B CN106555071 B CN 106555071B CN 201611088685 A CN201611088685 A CN 201611088685A CN 106555071 B CN106555071 B CN 106555071B
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- 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
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- 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 discloses a kind of method for preparing CNT/aluminium composite material in aluminium powder surface in situ catalysis gaseous carbon source, comprises the following steps：(1) be dispersant using Nickelous nitrate hexahydrate as catalyst, absolute ethyl alcohol, pure aluminium powder be that raw metal prepares precursor powder powder；(2) precursor powder is placed in vertical heater situ synthesizing carbon nanotubes/aluminium composite material：It is methane to be passed through carbon-source gas, and reducing gas is hydrogen, and protection gas is argon gas；Sintering temperature is 500~630 DEG C；Gaseous carbon sources grow carbon pipe under catalyst action, obtain the carbon nano tube enhanced aluminium base composite powder of growth in situ；Prepare CNT/aluminium block composite material.This method technique is simple, and cost is cheap, the carbon nanotube enhanced aluminium-based composite material prepared, method of its comprehensive mechanical property better than the outer addition addition CNT of tradition.
Description
Technical field
The present invention relates to a kind of method using powder metallurgy carbon nano-tube in situ/aluminium composite material, belong to powder
Last metallurgical technology field.
Background technology
Aluminium and its alloy are content highest metal class materials in the earth's crust, are steel is only second in commercial Application second largest
Metalloid material.The density of aluminium is low, only 2.7g/cm3, electrical and thermal conductivity performance is good, damping characteristics are good, be widely applied to
Automotive hub, Aero-Space branch framework, mechano-electronic and some civil areas.But the intensity of fine aluminium is relatively low, some high-strength
The field that degree requires fails to produce a desired effect.Meanwhile in the process in later stage, aluminium also needs to keep certain deformation energy
Power.Therefore, how to improve the intensity of aluminium and keep certain plasticity and toughness to turn into the focus of current research.In recent decades, it is more
Number researcher is to add different types of alloying element in aluminum substrate to prepare various section bars by the technique of melting and casting.
However, the regulation and control of content and inaccurate in adding procedure of these alloying elements, Partial Elements are difficult to add and costly.This
Outside, the addition of alloying element causes many problems be present in terms of the performance evaluation of material later stage.In recent ten years, people attempt again
Some enhancings are added in metallic matrix and mutually improve the performance of composite.But these traditional methods are always original to sacrifice
Based on some performances of material, and the aluminum matrix composite being prepared into by the method for original position vapour deposition can be maximum
Overcome this shortcoming.According to composite Materials Design rule (δc=(1-f) δm+fδp), reinforcing effect is being realized in the addition for strengthening phase
While, the weak point of matrix material can also be avoided, so as to obtain the aluminium of high-strength light.
CNT has largely been ground since last century, the nineties were found by the extensive concern of professional and expansion
Study carefully, begun to take shape now.In recent ten years, the carbon nano tube enhanced aluminium base composite wood prepared using CNT as reinforcement
The research of material increases and developed rapidly year by year.So far, most of researchs concentrate on additional method and prepare CNT enhancing aluminium
On based composites, block composite wood is prepared by techniques such as powder metallurgy, mechanical ball mill, molecular level mixing, casting smeltings
Material.But above method can cause the destruction of carbon nano tube structure unavoidably, while also it is difficult to ensure that CNT in matrix material
In it is dispersed.So this is also the bottleneck place studied at present.To sum up, how to solve CNT in the base equal
It is even scattered to promote the good interface cohesion of CNT and matrix and keep complete turn into of self structure currently to prepare carbon and receive
Where the focus of mitron reinforced aluminum matrix composites.
So far, most researchers are prepared for CNT increasing using the method added in CNT to aluminum substrate
Strong aluminum matrix composite.The method that the present invention uses the additional powder metallurgy of vertical heater in-situ growing carbon nano tube, first in aluminium powder table
Uniform growth CNT on face, after technique by cold moudling and hot extrusion, prepare that consistency is high, CNT is equal
Even scattered and good mechanical performance aluminum matrix composite.
The content of the invention
It is an object of the invention to provide a kind of side of easy powder metallurgy carbon nano-tube in situ/aluminium composite material
Method.The shortcomings that this method can effectively overcome the additional carbon nanotube enhanced aluminium-based composite material enhancing distributed mutually of tradition uneven,
This procedure is relatively easy, and obtained composite materials property is preferable.To achieve the above object, the present invention by with
Lower technical scheme is carried out：
A kind of method for preparing CNT/aluminium composite material in aluminium powder surface in situ catalysis gaseous carbon source, including it is following
Step：
(1) precursor powder is prepared
Be dispersant using Nickelous nitrate hexahydrate as catalyst, absolute ethyl alcohol, pure aluminium powder be raw metal, according to catalyst：
Metal dust：Absolute ethyl alcohol=1g：15g：(50-100) ml proportioning, it will match somebody with somebody in catalyst and metal dust injection absolute ethyl alcohol
Dispersed mixed solution is made；Then by solution, heating stirring to ethanol is evaporated to obtain precursor powder powder in water-bath
End；
(2) carbon nano-tube in situ/aluminium composite material
Precursor powder made from step (1) is placed in vertical heater situ synthesizing carbon nanotubes/aluminium composite material：It is passed through
Carbon-source gas are methane, and reducing gas is hydrogen, and protection gas is argon gas；Sintering temperature is 500~630 DEG C, the recovery time 0.5
~1.5h；Gaseous carbon sources grow carbon pipe under catalyst action, obtain the carbon nano tube enhanced aluminium base composite powder of growth in situ
End；
(3) CNT/aluminium block composite material is prepared
By the composite powder obtained in step (2) after mechanical ball mill technique it is cold-rolled sintered after hot extrusion molding prepare block
Body material.
Preferably, step 1) water bath heating temperature is 90 DEG C, and mixing time is 3 hours.Step 2) gas flow controls model
Enclose for 100~300ml/min of argon gas；50~200ml/min of hydrogen；20~50ml/min of methane；Step 3) in mechanical milling process,
Parameter is 200~500 revs/min, 0.5~8h of ball milling；In cold moudling and hot extrusion process, cold pressing pressure be 400~
500MPa, dwell time are 3~5min；In hot extrusion process, temperature is 400~550 DEG C, and pressure is 500~600MPa.
The present invention has advantages below：The method for directly using growth in situ first, makes gaseous carbon sources methane in aluminium powder table
Realize uniform growth in face.Secondly, simple using this method technique, cost is cheap, and the carbon nano tube enhanced aluminium base prepared is answered
Condensation material, method of its comprehensive mechanical property better than the outer addition addition CNT of tradition.
Brief description of the drawings
Fig. 1 a are the scanned photograph that CNT is generated after being reduced in embodiment 1.
Fig. 1 b are the scanned photograph that CNT is generated after being reduced in embodiment 2.
Fig. 1 c are the scanned photograph that CNT is generated after being reduced in embodiment 3.
Fig. 1 d are the transmission spectrum photo of powder after being reduced in embodiment 1.
Fig. 1 e are the transmission spectrum photo of powder after being reduced in embodiment 2.
Fig. 1 f are the transmission spectrum photo of powder after being reduced in embodiment 3.
Fig. 2 a are the photo after powder ball milling in embodiment 4.
Fig. 2 b are the photo after powder ball milling in embodiment 5.
Fig. 2 c are the photo after powder ball milling in embodiment 6.
Fig. 2 d are photo after powder ball milling in embodiment 10.
Fig. 3 is the stress strain curve of block materials in embodiment 7,8,9,10.
Fig. 4 a are the stretching fracture pattern of block materials in embodiment 7.
Fig. 4 b are the stretching fracture pattern of block materials in embodiment 8.
Fig. 4 c are the stretching fracture pattern of block materials in embodiment 9.
Fig. 4 d are the stretching fracture pattern of block materials in embodiment 10.
Embodiment
The present invention is further illustrated with reference to example, these examples are served only for the explanation present invention, are not intended to limit the present invention.
Embodiment 1
Be dispersant using Nickelous nitrate hexahydrate as catalyst, absolute ethyl alcohol, pure aluminium powder be raw metal, according to catalyst：
Metal dust：Absolute ethyl alcohol=1g：15g：(50-100) ml proportioning, it will match somebody with somebody in catalyst and metal dust injection absolute ethyl alcohol
Mixed solution is made.Ultrasonic 30min after magnetic agitation 1h, is then placed in heating stirring in water-bath by mixed solution.Temperature is set
It is set to 90 DEG C, mixing time 3h, takes out above-mentioned dried powder when ethanol volatilizees totally, above-mentioned powder is placed in vertical tubular furnace
Middle carry out reduction treatment.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow is set in 50~200ml/ to hydrogen
Min), the recovery time is 1~2h；After be passed through methane, gas flow is set in 20~50ml/min, and protective atmosphere is argon gas
(gas flow is set in 50~300ml/min), catalytic temperature is set as 600 DEG C, catalysis time 0.5h so that methane is urged
CNT is melted into, prepares CNT/aluminium composite powder.The scanned photograph of material as shown in Figure 1a, transmits photo after reduction
As shown in Figure 1 d.
Embodiment 2
Be dispersant using Nickelous nitrate hexahydrate as catalyst, absolute ethyl alcohol, pure aluminium powder be raw metal, according to catalyst：
Metal dust：Absolute ethyl alcohol=1g：15g：(50-100) ml proportioning, it will match somebody with somebody in catalyst and metal dust injection absolute ethyl alcohol
Mixed solution is made.Ultrasonic 30min after magnetic agitation 1h, is then placed in heating stirring in water-bath by mixed solution.Temperature is set
It is set to 90 DEG C, mixing time 3h, takes out above-mentioned dried powder when ethanol volatilizees totally, above-mentioned powder is placed in vertical tubular furnace
Middle carry out reduction treatment.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow is set in 50~200ml/ to hydrogen
Min), the recovery time is 1~2h；After be passed through methane, gas flow is set in 20~50ml/min, and protective atmosphere is argon gas
(gas flow is set in 50~300ml/min), catalytic temperature is set as 600 DEG C, catalysis time 1h so that methane is catalyzed
Into CNT, CNT/aluminium composite powder is prepared.As shown in Figure 1 b, transmission photo is such as the scanned photograph of material after reduction
Shown in Fig. 1 e.
Embodiment 3
Be dispersant using Nickelous nitrate hexahydrate as catalyst, absolute ethyl alcohol, pure aluminium powder be raw metal, according to catalyst：
Metal dust：Absolute ethyl alcohol=1g：15g：(50-100) ml proportioning, it will match somebody with somebody in catalyst and metal dust injection absolute ethyl alcohol
Mixed solution is made.Ultrasonic 30min after magnetic agitation 1h, is then placed in heating stirring in water-bath by mixed solution.Temperature is set
It is set to 90 DEG C, mixing time 3h, takes out above-mentioned dried powder when ethanol volatilizees totally, above-mentioned powder is placed in vertical tubular furnace
Middle carry out reduction treatment.Reduction temperature is set in 400 DEG C, and reducing atmosphere is that (gas flow is set in 50~200ml/ to hydrogen
Min), the recovery time is 1~2h；After be passed through methane, gas flow is set in 20~50ml/min, and protective atmosphere is argon gas
(gas flow is set in 50~300ml/min), catalytic temperature is set as 600 DEG C, catalysis time 2h so that methane is catalyzed
Into CNT, CNT/aluminium composite powder is prepared.As illustrated in figure 1 c, transmission photo is such as the scanned photograph of material after reduction
Shown in Fig. 1 f.
Embodiment 4
By steel ball：Composite powder (CNT/Al powder in case study on implementation 2) presses quality (g) ratio 15：1 proportioning is put into
Into ball grinder, argon gas is filled with as protective atmosphere.In planetary ball mill by high-energy ball milling (400 revs/min, ball milling
0.5h).Ball milling result is as shown in Figure 2 a.
Embodiment 5
By steel ball：Composite powder (CNT/Al powder in case study on implementation 2) presses quality (g) ratio 15：1 proportioning is put into
Into ball grinder, argon gas is filled with as protective atmosphere.In planetary ball mill by high-energy ball milling (400 revs/min, ball milling
2h).Ball milling result is as shown in Figure 2 b.
Embodiment 6
By steel ball：Composite powder (CNT/Al powder in case study on implementation 2) presses quality (g) ratio 15：1 proportioning is put into
Into ball grinder, argon gas is filled with as protective atmosphere.In planetary ball mill by high-energy ball milling (400 revs/min, ball milling
4h).Ball milling result is as shown in Figure 2 c.
Embodiment 7
By powder cold moudling after the ball milling of case study on implementation 4, pressure is set as 400~500MPa, the dwell time is 3~
5min, after by formed blocks vacuum-sintering, sintering temperature is 500 DEG C, and time 1h, protective atmosphere is argon gas.Then will sintering
Complete block carries out hot extrusion, and heating-up temperature is 400~550 DEG C, and squeeze pressure is 500~600MPa；Under universal testing machine
Its tensile property is tested, its tensile strength reaches 140MPa.Stress strain curve is as shown in No. 2 curves in Fig. 3, fracture apperance such as Fig. 4 a
It is shown.
Embodiment 8
CNT prepared by case study on implementation 5/aluminium composite powder cold moudling, pressure are set as 400~500MPa, protect
The pressure time is 3~5min, after by formed blocks vacuum-sintering, sintering temperature is 500 DEG C, and time 1h, protective atmosphere is argon gas.
The block sintered is then subjected to hot extrusion, heating-up temperature is 400~550 DEG C, and squeeze pressure is 500~600MPa；Ten thousand
Its tensile property can be tested under testing machine, its tensile strength reaches 280MPa.Stress strain curve is as shown in No. 3 curves in Fig. 3, fracture
Pattern is as shown in Figure 4 b.
Embodiment 9
CNT prepared by case study on implementation 6/aluminium composite powder cold moudling, pressure are set as 400~500MPa, protect
The pressure time is 3~5min, after by formed blocks vacuum-sintering, sintering temperature is 500 DEG C, and time 1h, protective atmosphere is argon gas.
The block sintered is then subjected to hot extrusion, heating-up temperature is 400~550 DEG C, and squeeze pressure is 500~600MPa；Ten thousand
Its tensile property can be tested under testing machine, its tensile strength reaches 240MPa.Stress strain curve is as shown in 4 curves 3 in Fig. 3, fracture
Pattern is as illustrated in fig. 4 c.
Embodiment 10 (blank control test)
By steel ball：Pure Al powder presses quality (g) ratio 15：1 proportioning is put into ball grinder, is filled with argon gas as protection gas
Atmosphere.Pass through high-energy ball milling (400 revs/min, ball milling 4h) in planetary ball mill；Scanning pattern after ball milling is as shown in Figure 2 d.
By the powder cold moudling after ball milling, pressure is set as 400~500MPa, and the dwell time is 3~5min, after formed blocks are true
Sky sintering, sintering temperature are 500 DEG C, and time 1h, protective atmosphere is argon gas.The block sintered is subjected to hot extrusion afterwards,
Heating-up temperature is 400~550 DEG C, and squeeze pressure is 500~600MPa；Its tensile property is tested under universal testing machine, it draws
It is 80MPa to stretch intensity.Stress strain curve is as shown in No. 1 curve in Fig. 3, and fracture apperance is as shown in figure 4d.
It can be seen from four stress strain curves in Fig. 3 when it is 1h (No. 3 curves) to be passed through the methane time, composite
Tensile strength reach peak value (280MPa), the tensile strength (82MPa) compared to the fine aluminium by ball milling is higher by 243%, extension
Rate also maintains nearly 13%, and unlikely decline is too many.The time length of ball milling can all influence the mechanical property of material.
Claims (4)
1. a kind of method for preparing CNT/aluminium composite material in aluminium powder surface in situ catalysis gaseous carbon source, including following step
Suddenly：
(1) precursor powder is prepared
Be dispersant using Nickelous nitrate hexahydrate as catalyst, absolute ethyl alcohol, pure aluminium powder be raw metal, according to catalyst：Metal
Powder：Absolute ethyl alcohol=1g：15g：(50-100) ml proportioning, it will be configured in catalyst and metal dust injection absolute ethyl alcohol
Dispersed mixed solution；Then by solution, heating stirring is evaporated to ethanol to obtain precursor powder in water-bath；
(2) carbon nano-tube in situ/aluminium composite material
Precursor powder made from step (1) is placed in vertical heater situ synthesizing carbon nanotubes/aluminium composite material：It is passed through carbon source
Gas is methane, and reducing gas is hydrogen, and protection gas is argon gas；Sintering temperature be 500~630 DEG C, the recovery time be 0.5~
1.5h；Gaseous carbon sources grow carbon pipe under catalyst action, obtain the carbon nano tube enhanced aluminium base composite powder of growth in situ；
(3) CNT/aluminium block composite material is prepared
By the composite powder obtained in step (2) after mechanical ball mill technique it is cold-rolled sintered after hot extrusion molding prepare block material
Material.
2. according to claim 1 prepare CNT/aluminium composite material in aluminium powder surface in situ catalysis gaseous carbon source
Method, it is characterised in that step 1) water bath heating temperature is 90 DEG C, and mixing time is 3 hours.
3. according to claim 1 prepare CNT/aluminium composite material in aluminium powder surface in situ catalysis gaseous carbon source
Method, it is characterised in that step 2) gas flow control range is 100~300ml/min of argon gas；50~200ml/min of hydrogen；
20~50ml/min of methane.
4. according to claim 1 prepare CNT/aluminium composite material in aluminium powder surface in situ catalysis gaseous carbon source
Method, it is characterised in that step 3) is in mechanical milling process, and parameter is 200~500 revs/min, 0.5~8h of ball milling；In cold moudling
In hot extrusion process, cold pressing pressure is 400~500MPa, and the dwell time is 3~5min；In hot extrusion process, temperature 400
~550 DEG C, pressure is 500~600MPa.
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| CN108817381A (en) * | 2018-05-14 | 2018-11-16 | 兰州交通大学 | A kind of low bulk flake graphite/carbon nanotube/aluminium composite material preparation method |
| CN108796259A (en) * | 2018-07-04 | 2018-11-13 | 湘潭大学 | A kind of preparation method of carbon nanotube enhancing Zn based composites |
| CN109338134A (en) * | 2018-09-08 | 2019-02-15 | 天津大学 | A kind of preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites |
| CN109663921B (en) * | 2019-01-24 | 2021-12-14 | 上海交通大学 | Composite material plate and preparation method thereof |
| CN110744045A (en) * | 2019-09-06 | 2020-02-04 | 西安交通大学 | Method for in-situ synthesis of carbon nano tube on surface of aluminum alloy spherical powder |
| CN112974795B (en) * | 2021-02-05 | 2022-07-12 | 中国人民解放军陆军装甲兵学院 | Composite powder for additive manufacturing and remanufacturing and preparation method thereof, and metal-based composite forming layer and preparation method thereof |
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| CN102424919A (en) * | 2011-12-05 | 2012-04-25 | 天津大学 | Method for preparing carbon nanotube reinforced aluminum-based composite material |
| CN103276322B (en) * | 2013-06-17 | 2015-10-07 | 哈尔滨工业大学 | A kind of preparation method of In-situ grown carbon-nanotube-reinaluminum-base aluminum-base solder |
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