CN107442769A - A kind of high volume fraction carbon nano-pipe aluminium alloy compound dusty material and preparation method - Google Patents
A kind of high volume fraction carbon nano-pipe aluminium alloy compound dusty material and preparation method Download PDFInfo
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- CN107442769A CN107442769A CN201710691020.1A CN201710691020A CN107442769A CN 107442769 A CN107442769 A CN 107442769A CN 201710691020 A CN201710691020 A CN 201710691020A CN 107442769 A CN107442769 A CN 107442769A
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 54
- 239000000463 material Substances 0.000 title claims abstract description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 150000001875 compounds Chemical class 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 64
- 238000001238 wet grinding Methods 0.000 claims abstract description 16
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims description 47
- 238000000227 grinding Methods 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 9
- 238000003801 milling Methods 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 7
- 239000002079 double walled nanotube Substances 0.000 claims description 5
- 239000002048 multi walled nanotube Substances 0.000 claims description 5
- 239000002109 single walled nanotube Substances 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 18
- 239000002245 particle Substances 0.000 abstract description 8
- 229910045601 alloy Inorganic materials 0.000 abstract description 5
- 239000000956 alloy Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract 1
- 239000004677 Nylon Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 229920001778 nylon Polymers 0.000 description 9
- 230000002787 reinforcement Effects 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000002041 carbon nanotube Substances 0.000 description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
Classifications
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- B22F1/0003—
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
A kind of high volume fraction carbon nano-pipe aluminium alloy compound powder and preparation method, it is characterised in that：Its preparing raw material is CNT and Al alloy powder；Preparation method is first, CNT wet-milling is made into its scattered opening, then wet-milling, drying are carried out after Al alloy powder is mixed with CNT again, the dried powder after drying is finally subjected to further high-energy ball milling, finally gives required CNT aluminium alloy compound powder.It is provided by the invention：CNT can be efficiently entering inside alloy powder particles in the composite powder of the CNT of high-volume fractional 1 ~ 2% and Al alloy powder, form a kind of high volume fraction carbon nano-pipe aluminium alloy compound dusty material.
Description
Technical field
The present invention relates to a kind of composite powder material technical field, especially a kind of high volume fraction carbon nano-pipe（CNT）
Aluminium alloy compound dusty material and preparation method thereof.
Background technology
Aluminum matrix composite has that isotropism is high, density is low, higher than modulus of elasticity, specific strength is high, high temperature resistant, resistance to tired
A series of excellent specific properties such as labor, low bulk, high heat conduction, high reliability, and prepare, process industrial art performance it is good, the base that can be relied on
Plinth industrial might is strong, civil-military inosculation is good, has in major areas such as Aero-Space, advanced weaponry, information instrument, communications and transportation
Wide application background and irreplaceable effect.The nanoscale reinforcement of even dispersion distribution, gained are introduced in aluminum substrate
Composite can often show more preferably mechanical property and conduction, heat conduction, wear-resisting, anti-corrosion, high temperature resistant, antioxygen
The performances such as change.CNT（CNT）It is to prepare aluminum matrix composite to manage the most with performances such as excellent mechanics, electricity, calorifics
One of reinforcement thought, it has also become the focus of research.
Traditional composite powder preparation method, nanometer reinforcement are only attached to the surface of aluminum substrate, prepare aluminum-base composite material
A nanometer reinforcement is caused to be reunited during material.Therefore nanoscale reinforcement exists in content compared with Gao Shiyi with aggregated form, reduces
Enhancing effect, and can deteriorate plasticity and toughness.In addition, also there is be difficult to form effective interface cohesion with aluminum substrate for CNT
Problem, it not is very big that the performance of prepared composite, which improves, especially in terms of mechanical property, is far from reaching preferable
Value.Thus, the limitation of original technology how is broken through, finds more preferable preparation method to improve the performance of aluminum matrix composite, is
The important development direction of composite, and this area forward position scholar endeavour the subject matter of research always.
Main innovation of the present invention is to prepare high-volume fractional（1~2%）It is prepared by CNT aluminium alloy compound powder, tradition
Method is only capable of preparing the CNT that volume fraction is 0.2%.With this high volume fraction carbon nano-pipe aluminium alloy compound powder system
Standby composite material reinforcement body（CNT）It can be uniformly dispersed, be obviously improved relative to conventional composite materials property.
The content of the invention
The present invention is only capable of preparing the CNT enhancing composite powder that volume fraction is 0.2% for existing preparation method
Material and the problem of cause its performance to be difficult to further improve, invent a kind of high volume fraction carbon nano-pipe aluminium alloy compound powder
Material and preparation method thereof, it passes through " CNT wet-milling-CNT and Al alloy powder wet-milling-CNT and aluminium alloy
Powder high-energy ball milling " prepares composite powder material, and by adding the CNT of high-volume fractional, preferable carbon nanometer is prepared
Pipe aluminium alloy compound dusty material.
One of technical scheme is：
A kind of high volume fraction carbon nano-pipe aluminium alloy compound dusty material, it is characterized in that it is by CNT and Al alloy powder
Composition, CNT and Al alloy powder are calculated with percent by volume, wherein, CNT：1 ~ 2%, surplus is Al alloy powder
End, the percent by volume sum of each component is 100%.
Described CNT is single-walled carbon nanotube, double-walled carbon nano-tube or multi-walled carbon nanotube.
The purity of described CNT is not less than 99.0%.
The two of technical scheme are：
A kind of preparation method of high volume fraction carbon nano-pipe aluminium alloy compound dusty material, it is characterized in that it includes following step
Suddenly：
（1）The wet-milling of CNT：The CNT for taking volume fraction to be 1 ~ 2%, is put into ball grinder, is placed in ball mill with one
Determine ball milling parameter wet-milling so that the CNT fully group of solution, opening；
（2）The Wet blend-milling of Al alloy powder and CNT：Take Al alloy powder and step（1）The CNT of middle wet-milling is carried out
Wet blend-milling so that mixed powder is fully dispersed, and the mixed powder after ball milling is placed in drying baker into the xeraphium dried, mixed
End；
（3）High-energy ball milling mixed-powder：By step（2）The dried powder of obtained mixing is put into ball grinder, is placed in ball mill
Ball milling so that CNT can be uniformly distributed in inside Al alloy powder, obtains high volume fraction carbon nano-pipe aluminium alloy and answers
Close dusty material.
Described CNT is single-walled carbon nanotube, double-walled carbon nano-tube or multi-walled carbon nanotube, and CNT
Purity is not less than 99.0%.
Step（1）With（2）Described in the ball-milling technology of wet-milling be：75% alcoholic media, ratio of grinding media to material（6~8）：1,250 ±
50r/min 10 ~ 12h of ball milling, 10 ± 5min is shut down per ball milling 1h.
Step（2）Described drying temperature is 90 ~ 110 DEG C, and drying time is 4 ~ 8h.
Step（3）The ball-milling technology of described high-energy ball milling is：Ratio of grinding media to material（6~8）：1,300 ± 50r/min ball millings 12 ~
24h, 10 ± 5min is shut down per ball milling 1h.
The beneficial effects of the invention are as follows：
（1）The present invention innovatively proposes a kind of preparation method of high volume fraction carbon nano-pipe aluminium alloy compound dusty material,
Make CNT is scattered to open by wet-milling, in the composite powder stage, pass through Wet blend-milling and further high-energy ball milling so that increase
Strong body CNT is forced scattered and is efficiently entering inside alloy powder particles.
（2）The preparation method of the present invention can make increasing compared to the composite powder material commonly without further high-energy ball milling
Strong body CNT is dispersed in inside alloyed powder.
（3）The preparation method of the present invention, it is 2% CNT that can prepare high-volume fractional, and tradition prepares dusty material
Method in carbon nanotube by volume fraction only have 0.2%.
（3）A kind of preparation method operation letter of high volume fraction carbon nano-pipe aluminium alloy compound powder provided by the invention
Single, easily realization, economical.
Brief description of the drawings
Fig. 1 is the Technology Roadmap of the preparation method of the present invention.
Fig. 2 is the SEM shape appearance figures after being prepared in the embodiment of the present invention.
Fig. 3 is the SEM shape appearance figures for the CNT observed after being prepared in the embodiment of the present invention.
Fig. 4 is the SEM shape appearance figures prepared in comparative example of the present invention.
Embodiment
The embodiment of the present invention is described in detail with reference to the accompanying drawings and examples, but the present invention not only limits
In embodiment.
Embodiment one.
As shown in Fig. 2 ~ 3.
A kind of high volume fraction carbon nano-pipe is the preparation method of 2% aluminium alloy compound powder：
First, 0.44g CNT is configured（Can be in single-walled carbon nanotube, double-walled carbon nano-tube or multi-walled carbon nanotube
One or more of combinations, similarly hereinafter）, wherein carbon nanotube by volume fraction 2%, i.e. mass fraction 1.1wt.%（0.44g）, according to
Ratio of grinding media to material 6:1, which first weighs 2.64g agate balls, is placed in 500 ml nylon ball grinders, then CNT is placed in nylon tank, is connect
The alcohol for inserting that purity is 95%, is sealed；
Then, ball grinder is arranged on planetary ball mill, starts ball milling, ball milling parameter is arranged to 250 r/min, and ball milling 1h stops
The min of machine 10 ± 5, Ball-milling Time are 12 h；
Secondly, configuration Al alloy powder 39.56g（Particle diameter≤10 micron, similarly hereinafter）, according to ratio of grinding media to material 6:1 weighs 237.36g agate balls
It is placed in above-mentioned wet-milling ball grinder, inserts the alcohol that concentration is 95%, with 0.44g CNT Wet blend-millings, ball milling parameter is set
10 ± 5min is shut down, drying is taken out after ball milling at least 12 ± 1 h for 250 r/min, ball milling 1h；
Afterwards, dry mixed powder and agate ball are again placed in carrying out high-energy ball milling in nylon ball grinder, ball milling parameter is set
10 ± 5 min are shut down, powder in ball grinder is taken out after 12 ± 1h of ball milling, that is, obtains high volume integral for 300 r/min, ball milling 1h
Number CNT aluminium alloy compound dusty material；
2% high volume fraction carbon nano-pipe aluminium alloy compound powder is made using above-mentioned steps, Fig. 2 is the SEM patterns after preparing
Figure, analyzes from figure and draws, CNT can be uniformly dispersed in inside alloyed powder；Fig. 3 is the shape for the CNT that observation obtains
Looks figure, it can be seen that CNT can be well dispersed in alloyed powder, i.e., high-volume fractional carbon nanometer is successfully made
Pipe aluminium alloy compound dusty material.
Comparative example
As shown in Figure 4.
The present embodiment preparation method is similar to embodiment one, and difference is that preparation method does not have the high energy of final step
Ball milling, i.e. " CNT wet-milling-CNT and Al alloy powder wet-milling "
Fig. 4 is the SEM shape appearance figures that the preparation method obtains, and is found through analysis, and 2% CNT is with after Al alloy powder wet-milling, strengthening
Body is enriched in alloyed powder particle surface, fails to be efficiently entering inside alloy powder particles, and fail obtained composite powder material.
Embodiment and comparative example contrast are found that the high-energy ball milling of final step is committed step in preparation method, is lacked
High-energy ball milling, reinforcement CNT can not be efficiently entering inside alloy powder particles, be only enriched in alloyed powder particle surface；And pass through
Reinforcement is forced scattered and is efficiently entering inside alloy powder particles after further high-energy ball milling, and it is equal to form reinforcement CNT
The even high quality composite powder being dispersed in inside alloyed powder.
Embodiment two.
A kind of high volume fraction carbon nano-pipe is the preparation method of 1% aluminium alloy compound powder：
First, 0.22g CNT, wherein carbon nanotube by volume fraction 1%, i.e. mass fraction 0.55wt.% are configured
（0.22g）, according to ratio of grinding media to material 8:1, which first weighs 1.76g agate balls, is placed in 500 ml nylon ball grinders, then CNT is placed in
In nylon tank, the alcohol that purity is 95% is then inserted, is sealed；
Then, ball grinder is arranged on planetary ball mill, starts ball milling, ball milling parameter is arranged to 250 r/min, and ball milling 1h stops
The min of machine 10 ± 5, Ball-milling Time are 12 ± 1 h；
Secondly, Al alloy powder 39.78g is configured, according to ratio of grinding media to material 8:1 weighing 318.24g agate balls are placed in above-mentioned wet-milling ball grinder
In, the alcohol that concentration is 95% is inserted, with 0.22g CNT Wet blend-millings, ball milling parameter is arranged to 250 ± 50r/min, ball
Grind 1h and shut down 10 ± 5min, drying is taken out after ball milling at least 12 ± 1 h；
Afterwards, dry mixed powder and agate ball are again placed in carrying out high-energy ball milling in nylon ball grinder, ball milling parameter is set
10 ± 5 min are shut down, powder in ball grinder is taken out after 12 ± 1h of ball milling, that is, obtains high body for 300 ± 50 r/min, ball milling 1h
Fraction CNT aluminium alloy compound dusty material；
1% high volume fraction carbon nano-pipe aluminium alloy compound powder is made using above-mentioned steps, SEM shape appearance figures and Fig. 2 after preparation
Approximation, CNT also can be uniformly dispersed in inside alloyed powder；The shape appearance figure of CNT is also close with Fig. 3, can from figure
To find out, CNT can be well dispersed in alloyed powder, i.e., high volume fraction carbon nano-pipe aluminium alloy compound is successfully made
Dusty material.
Embodiment three.
A kind of high volume fraction carbon nano-pipe is the preparation method of 1.5% aluminium alloy compound powder：
First, 0.33g CNT, wherein carbon nanotube by volume fraction 1.5%, i.e. mass fraction 0.83wt.% are configured
（0.33g）, according to ratio of grinding media to material 7:1, which first weighs 2.31g agate balls, is placed in 500 ml nylon ball grinders, then CNT is placed in
In nylon tank, the alcohol that purity is 95% is then inserted, is sealed；
Then, ball grinder is arranged on planetary ball mill, starts ball milling, ball milling parameter is arranged to 250 ± 50 r/min, ball milling
1h shuts down 10 ± 5 min, and Ball-milling Time is 12 ± 1 h；
Secondly, Al alloy powder 39.67g is configured, according to ratio of grinding media to material 7:1 weighing 277.69g agate balls are placed in above-mentioned wet-milling ball grinder
In, the alcohol that concentration is 95% is inserted, with 0.33g CNT Wet blend-millings, ball milling parameter is arranged to 250 ± 50r/min, ball
Grind 1h and shut down 10 ± 5min, drying is taken out after ball milling at least 12 ± 1 h；
Afterwards, dry mixed powder and agate ball are again placed in carrying out high-energy ball milling in nylon ball grinder, ball milling parameter is set
10 ± 5 min are shut down, powder in ball grinder is taken out after 12 ± 1h of ball milling, that is, obtains high body for 300 ± 50 r/min, ball milling 1h
Fraction CNT aluminium alloy compound dusty material；
1.5% high volume fraction carbon nano-pipe aluminium alloy compound powder is made using above-mentioned steps, the SEM shape appearance figures after preparation with
Fig. 2 is approximate, and CNT also can be uniformly dispersed in inside alloyed powder；The shape appearance figure of CNT is also close with Fig. 3, from figure
As can be seen that CNT can be well dispersed in alloyed powder, i.e., high volume fraction carbon nano-pipe aluminium alloy is successfully made and answers
Close dusty material.
Part that the present invention does not relate to is same as the prior art or can be realized using prior art.
Claims (8)
- A kind of 1. high volume fraction carbon nano-pipe aluminium alloy compound dusty material, it is characterized in that it is by CNT and Al alloy powder End composition, CNT and Al alloy powder are calculated with percent by volume, wherein, CNT：1 ~ 2%, surplus is aluminium alloy Powder, the percent by volume sum of each component is 100%.
- 2. high volume fraction carbon nano-pipe aluminium alloy compound dusty material according to claim 1, it is characterized in that described CNT is single-walled carbon nanotube, double-walled carbon nano-tube or multi-walled carbon nanotube.
- 3. high volume fraction carbon nano-pipe aluminium alloy compound dusty material according to claim 1 or 2, it is characterized in that described CNT purity be not less than 99.0%.
- 4. a kind of preparation method of the high volume fraction carbon nano-pipe aluminium alloy compound dusty material described in claim 1, it is special Sign is that it comprises the following steps：（1）The wet-milling of CNT：The CNT for taking volume fraction to be 1 ~ 2%, is put into ball grinder, is placed in ball mill with one Determine ball milling parameter wet-milling so that the CNT fully group of solution, opening；（2）The Wet blend-milling of Al alloy powder and CNT：Take Al alloy powder and step（1）The CNT of middle wet-milling is carried out Wet blend-milling so that mixed powder is fully dispersed, and the mixed powder after ball milling is placed in drying baker into the xeraphium dried, mixed End；（3）High-energy ball milling mixed-powder：By step（2）The dried powder of obtained mixing is put into ball grinder, is placed in ball mill Ball milling so that CNT can be uniformly distributed in inside Al alloy powder, obtains high volume fraction carbon nano-pipe aluminium alloy and answers Close dusty material.
- 5. preparation method according to claim 4, it is characterized in that described CNT is single-walled carbon nanotube, double-walled carbon Nanotube or multi-walled carbon nanotube, and the purity of CNT is not less than 99.0%.
- 6. preparation method according to claim 4, it is characterized in that step（1）With（2）Described in the ball-milling technology of wet-milling be： 75% alcoholic media, ratio of grinding media to material（6~8）：1,250 ± 50r/min, 10 ~ 12h of ball milling, 10 ± 5min is shut down per ball milling 1h.
- 7. preparation method according to claim 4, it is characterized in that step（2）Described drying temperature is 90 ~ 110 DEG C, is dried The dry time is 4 ~ 8h.
- 8. preparation method according to claim 4, it is characterized in that step（3）The ball-milling technology of described high-energy ball milling is： Ratio of grinding media to material（6~8）：1,300 ± 50r/min, 12 ~ 24h of ball milling, 10 ± 5min is shut down per ball milling 1h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103789564A (en) * | 2014-01-23 | 2014-05-14 | 上海交通大学 | Powder metallurgy preparation method of carbon nanotube reinforced aluminum alloy composite material |
| CN103911566A (en) * | 2014-03-11 | 2014-07-09 | 上海交通大学 | Powder metallurgy preparation method of carbon nanotube reinforced aluminium alloy composite material |
| CN106363185A (en) * | 2016-08-26 | 2017-02-01 | 上海交通大学 | Powder metallurgy preparation method of nanophase/metal composite powder and block material thereof |
-
2017
- 2017-08-14 CN CN201710691020.1A patent/CN107442769A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103789564A (en) * | 2014-01-23 | 2014-05-14 | 上海交通大学 | Powder metallurgy preparation method of carbon nanotube reinforced aluminum alloy composite material |
| CN103911566A (en) * | 2014-03-11 | 2014-07-09 | 上海交通大学 | Powder metallurgy preparation method of carbon nanotube reinforced aluminium alloy composite material |
| CN106363185A (en) * | 2016-08-26 | 2017-02-01 | 上海交通大学 | Powder metallurgy preparation method of nanophase/metal composite powder and block material thereof |
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Application publication date: 20171208 |