CN102268580A - Method for preparing boron-doped carbon nanotube reinforced magnesium matrix composite material - Google Patents
Method for preparing boron-doped carbon nanotube reinforced magnesium matrix composite material Download PDFInfo
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- CN102268580A CN102268580A CN 201110220133 CN201110220133A CN102268580A CN 102268580 A CN102268580 A CN 102268580A CN 201110220133 CN201110220133 CN 201110220133 CN 201110220133 A CN201110220133 A CN 201110220133A CN 102268580 A CN102268580 A CN 102268580A
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Abstract
The invention relates to a method for preparing a boron-doped carbon nanotube reinforced magnesium matrix composite material, and belongs to a magnesium matrix composite material preparation technology. The method comprises the following steps of: performing boron doping on carbon nanotubes by using B2O3 as a boron source; dispersing the boron-doped carbon nanotubes by using a 3-(N-N-dimethylmyristylammonio)propanesulfonate amphoteric surfactant; mixing the dispersed boron-doped carbon nanotubes with magnesium, and performing compression moulding and primary sintering; and repressing and secondarily sintering a magnesium matrix composite material to obtain the boron-doped carbon nanotube reinforced magnesium matrix composite material. The invention has the advantages that: the mechanical properties of the boron-doped carbon nanotube reinforced magnesium matrix composite material are improved, and the preparation process for the magnesium matrix composite material is easy to operate. The prepared high strength magnesium matrix composite material can be widely applied to the fields such as aerospace, automobiles and the like.
Description
Technical field
The present invention relates to a kind of boron doped carbon nanotube and strengthen method of preparing magnesium-based composite material, belong to the technology of preparing of magnesium base composite material.
Background technology
Magnesium base composite material belongs to a kind of of light metal matrix material, and its principal feature is that density is low, specific tenacity, specific rigidity height, also has good shock-resistance, high thermal resistance, wear resistance, good damping performance and good dimensional stability etc. simultaneously.In addition, also have hydrogen storage property and electromagnetic shielding etc., being outstanding structure of a class and functional materials, also is to be hopeful one of composite applications most in the current high-technology field, in fields such as aerospace, war products manufacturing, Electronic Packaging and automobile great application prospect is arranged.Therefore, magnesium base composite material becomes one of light metal-based composite study focus.
Carbon nanotube intensity is high, and average Young's modulus can reach 1～1.8TPa, and 100 times of the chances are steel are 20 times of carbon fiber, and flexural strength can reach 14.2GPa, and the strain energy of depositing reaches 100keV, and interlaminar shear strength reaches 500MPa.Carbon nanotube is as one dimension hollow molecules material, and density has only 1/6 of steel, and weight is 1/2 of carbon fiber.Carbon nanotube relies on its high specific tenacity and specific rigidity, and extremely low density and axial thermal expansion coefficient and unique conduction and thermal conductivity become the optimal wild phase of matrix material.
When preparing magnesium base composite material as wild phase with carbon nanotube, because the CNTs of complete structure is more stable, especially with during the light metal interface of no d electronics combines inertia appears, cause the weak interface bond strength that gets, and weak interface bond strength meeting havoc performance of composites, therefore, the interface bond strength of raising carbon nanotube and magnesium base is the key of the carbon nanotube enhancing magnesium base composite material of processability excellence.At present, be coating, coating, defective and doping etc. in metal material field to carbon nanotube modification mode commonly used.These technologies have solved the load transmission such as the CNTs/ high polymer composite material, the reunion and the associativity of carbon nanotube, are a kind of effective meanss.Wherein, the boron doped carbon nanometer pipe generally adopts method preparations such as growth in situ, high temperature gas phase method, yet the research of boron doped carbon nanometer pipe concentrates on its physicals and electric property at present, and its performance that strengthens magnesium base composite material is not reported as yet.
To sum up, how adopting the preparation technology of simple and stable, improve the interface bond strength of carbon nanotube and magnesium matrix, is that the carbon nanotube of research and development preparation at present strengthens the subject matter that magnesium base composite material faces.
Summary of the invention
Purpose of the present invention provides a kind of boron doped carbon nanotube to strengthen method of preparing magnesium-based composite material.Preparation is simple for this method, the intensity height of prepared matrix material.
The present invention is achieved by the following technical solutions, and a kind of boron doped carbon nanotube strengthens method of preparing magnesium-based composite material, and its embodiment comprises following process:
1) with B
2O
3As the boron source, it is 10: 1 by the atomic ratio of boron atom and carbon atom.With B
2O
3Put into Noah's ark bottom, the coated carbon nanotube places tube furnace with Noah's ark more in the above, is warming up to 1100-1300 ℃ with the temperature rise rate of 10 ℃/min, and insulation is 3-5 hour under the atmosphere of argon gas;
2) adopt three-sulfopropyl tetradecyl diformazan trimethyl-glycine surface bi ion active agent that the boron doped carbon nanometer pipe is disperseed.The mass ratio of dispersion agent and boron doped carbon nanometer pipe is 1: 10, dispersion agent is dissolved in the 200-300ml Virahol under 60 ℃ of temperature, the boron doped carbon nanometer pipe was joined in the gained solution ultrasonic agitation 30 minutes, the mass ratio of pressing boron doped carbon nanometer pipe and magnesium is (0.1-1.5): (99.9-98.5), to cross 200 purpose magnesium powder again joins in the gained solution, mixed 20-40 minute, suction filtration then, dry down and grind evenly at temperature 50-80 ℃, obtain the composite powder of boron doped carbon nanometer pipe with magnesium;
3) with step 2) composite powder of gained suppressed under pressure 500-700MPa 2-3 minute, having obtained diameter is the block of the matrix material of 20mm, temperature rise rate with 10 ℃/min is warming up to 500-600 ℃, under the protective atmosphere of argon gas, carried out sintering 1-3 hour, then the block that obtains was carried out multiple pressure 2-3 minute under pressure 600-750MPa, temperature rise rate with 10 ℃/min is warming up to 550-650 ℃, reburns to tie 1-3 hour under the protective atmosphere of argon gas; The cooling room temperature obtains the boron doped carbon nanometer pipe and strengthens magnesium base composite material.
The present invention has the following advantages: under the lower situation of the atom doped ratio of boron, the mechanical property of matrix material has obtained improvement by a relatively large margin, when the atom doped ratio of boron reaches 3.1%, and when boron doped carbon nanometer pipe content was 1.5wt.%, the compressive strength of prepared magnesium base composite material had improved 15%.Preparation process of the present invention is easy to operate.Prepared high-strength magnesium based composites can be widely used in fields such as aerospace and automobile.
Description of drawings
The XPS collection of illustrative plates of the boron doped carbon nanometer pipe that Fig. 1 makes for the embodiment of the invention one, two, three.
The boron doped carbon nanometer pipe content that Fig. 2 makes for the embodiment of the invention one is that the stress under compression strain curve (b) of magnesium base composite material of 0.1wt.% and the content of carbon nanotubes that comparative example one makes are the stress under compression strain curve (a) of the magnesium base composite material of 0.1wt.%.
The boron doped carbon nanometer pipe content that Fig. 3 makes for the embodiment of the invention two is that the stress under compression strain curve (b) of magnesium base composite material of 0.5wt.% and the content of carbon nanotubes that comparative example two makes are the stress under compression strain curve (a) of the magnesium base composite material of 0.5wt.%.
The boron doped carbon nanometer pipe content that Fig. 4 makes for the embodiment of the invention three is that the stress under compression strain curve (b) of magnesium base composite material of 1.5wt.% and the content of carbon nanotubes that comparative example three makes are the stress under compression strain curve (a) of the magnesium base composite material of 1.5wt.%.
Embodiment
Embodiment one
With 3.5gB
2O
3Put into Noah's ark bottom, cover the 0.12g carbon nanotube in the above, Noah's ark is placed tube furnace, be warming up to 1150 ℃ of temperature with the temperature rise rate of 10 ℃/min, insulation is 4 hours under the atmosphere of argon gas; 0.001g three-sulfopropyl tetradecyl diformazan trimethyl-glycine is dissolved in the 200ml Virahol under 60 ℃ of temperature, then 0.01g boron doped carbon nanometer pipe was joined in the gained solution ultrasonic 30 minutes, 9.99g being crossed 200 purpose magnesium powder joins in the gained solution again, ultrasonic agitation 30 minutes, the mixing solutions of gained is carried out suction filtration and dry for 60 ℃, and grind evenly in temperature; The composite powder that makes was suppressed under pressure 550MPa 3 minutes, and having obtained diameter is the block of the matrix material of 20mm; Temperature rise rate with 10 ℃/min is warming up to 550 ℃ of temperature, under the protective atmosphere of argon gas, carried out sintering 1 hour, then the block that obtains was carried out multiple pressure 3 minutes under pressure 700MPa, temperature rise rate with 10 ℃/min is warming up to 600 ℃ of temperature, reburns to tie 2 hours under the protective atmosphere of argon gas; Be to carry out hot extrusion under 16: 1 the condition in 350 ℃ of temperature, extrusion ratio with the block that makes magnesium base composite material, obtaining diameter is the magnesium base composite material bar of 5mm.
Embodiment two
With 3.5gB
2O
3Put into Noah's ark bottom, cover the 0.12g carbon nanotube in the above, Noah's ark is placed tube furnace, be warming up to 1150 ℃ of temperature with the temperature rise rate of 10 ℃/min, insulation is 4 hours under the atmosphere of argon gas; 0.005g three-sulfopropyl tetradecyl diformazan trimethyl-glycine is dissolved in the 200ml Virahol under 60 ℃ of temperature, then 0.05g boron doped carbon nanometer pipe was joined in the gained solution ultrasonic 30 minutes, 9.95g being crossed 200 purpose magnesium powder joins in the gained solution again, ultrasonic agitation 30 minutes, the mixing solutions of gained is carried out suction filtration and dry for 60 ℃, and grind evenly in temperature; The composite powder that makes was suppressed under pressure 550MPa 3 minutes, and having obtained diameter is the block of the magnesium base composite material of 20mm; Temperature rise rate with 10 ℃/min is warming up to 550 ℃ of temperature, under the protective atmosphere of argon gas, carried out sintering 1 hour, then the block that obtains was carried out multiple pressure 3 minutes under pressure 700MPa, temperature rise rate with 10 ℃/min is warming up to 600 ℃ of temperature, reburns to tie 2 hours under the protective atmosphere of argon gas; Be to carry out hot extrusion under 16: 1 the condition in 350 ℃ of temperature, extrusion ratio with the block that makes magnesium base composite material, obtaining diameter is the magnesium base composite material bar of 5mm.
Embodiment three
With 3.5gB
2O
3Put into Noah's ark bottom, cover the 0.12g carbon nanotube in the above, Noah's ark is placed tube furnace, be warming up to 1150 ℃ of temperature with the temperature rise rate of 10 ℃/min, insulation is 4 hours under the atmosphere of argon gas; 0.015g three-sulfopropyl tetradecyl diformazan trimethyl-glycine is dissolved in the 200ml Virahol under 60 ℃ of temperature, then 0.15g boron doped carbon nanometer pipe was joined in the gained solution ultrasonic 30 minutes, 9.85g being crossed 200 purpose magnesium powder joins in the gained solution again, ultrasonic agitation 30 minutes, the mixing solutions of gained is carried out suction filtration and dry for 60 ℃, and grind evenly in temperature; The composite powder that makes was suppressed under pressure 550MPa 3 minutes, and having obtained diameter is the block of the magnesium base composite material of 20mm; Temperature rise rate with 10 ℃/min is warming up to 550 ℃ of temperature, under the protective atmosphere of argon gas, carried out sintering 1 hour, then the block that obtains was carried out multiple pressure 3 minutes under pressure 700MPa, temperature rise rate with 10 ℃/min is warming up to 600 ℃ of temperature, reburns to tie 2 hours under the protective atmosphere of argon gas; Be to carry out hot extrusion under 16: 1 the condition in 350 ℃ of temperature, extrusion ratio with the block that makes magnesium base composite material, obtaining diameter is the magnesium base composite material bar of 5mm.
The comparative example one
0.001g three-sulfopropyl tetradecyl diformazan trimethyl-glycine is dissolved in the 200ml Virahol under 60 ℃ of temperature, then the 0.01g carbon nanotube was joined in the gained solution ultrasonic 30 minutes, 9.99g being crossed 200 purpose magnesium powder joins in the gained solution again, ultrasonic agitation 30 minutes, the mixing solutions of gained is carried out suction filtration and dry for 60 ℃, and grind evenly in temperature; The composite powder that makes was suppressed under pressure 550MPa 3 minutes, and having obtained diameter is the block of the magnesium base composite material of 20mm; Temperature rise rate with 10 ℃/min is warming up to 550 ℃ of temperature, under the protective atmosphere of argon gas, carried out sintering 1 hour, then the block that obtains was carried out multiple pressure 3 minutes under pressure 700MPa, temperature rise rate with 10 ℃/min is warming up to 600 ℃ of temperature, reburns to tie 2 hours under the protective atmosphere of argon gas; Be to carry out hot extrusion under 16: 1 the condition in 350 ℃ of temperature, extrusion ratio with the block that makes magnesium base composite material, obtaining diameter is the magnesium base composite material bar of 5mm.
The comparative example two
0.005g three-sulfopropyl tetradecyl diformazan trimethyl-glycine is dissolved in the 200ml Virahol under 60 ℃ of temperature, then the 0.05g carbon nanotube was joined in the gained solution ultrasonic 30 minutes, 9.95g being crossed 200 purpose magnesium powder joins in the gained solution again, ultrasonic agitation 30 minutes, the mixing solutions of gained is carried out suction filtration and dry for 60 ℃, and grind evenly in temperature; The composite powder that makes was suppressed under pressure 550MPa 3 minutes, and having obtained diameter is the block of the magnesium base composite material of 20mm; Temperature rise rate with 10 ℃/min is warming up to 550 ℃ of temperature, under the protective atmosphere of argon gas, carried out sintering 1 hour, then the block that obtains was carried out multiple pressure 3 minutes under pressure 700MPa, temperature rise rate with 10 ℃/min is warming up to 600 ℃ of temperature, reburns to tie 2 hours under the protective atmosphere of argon gas; Be to carry out hot extrusion under 16: 1 the condition in 350 ℃ of temperature, extrusion ratio with the block that makes magnesium base composite material, obtaining diameter is the magnesium base composite material bar of 5mm.
The comparative example three
0.015g three-sulfopropyl tetradecyl diformazan trimethyl-glycine is dissolved in the 200ml Virahol under 60 ℃ of temperature, then the 0.15g carbon nanotube was joined in the gained solution ultrasonic 30 minutes, 9.85g being crossed 200 purpose magnesium powder joins in the gained solution again, ultrasonic agitation 30 minutes, the mixing solutions of gained is carried out suction filtration and dry for 60 ℃, and grind evenly in temperature; The composite powder that makes was suppressed under pressure 550MPa 3 minutes, and having obtained diameter is the block of the magnesium base composite material of 20mm; Temperature rise rate with 10 ℃/min is warming up to 550 ℃ of temperature, under the protective atmosphere of argon gas, carried out sintering 1 hour, then the block that obtains was carried out multiple pressure 3 minutes under pressure 700MPa, temperature rise rate with 10 ℃/min is warming up to 600 ℃ of temperature, reburns to tie 2 hours under the protective atmosphere of argon gas; Be to carry out hot extrusion under 16: 1 the condition in 350 ℃ of temperature, extrusion ratio with the block that makes magnesium base composite material, obtaining diameter is the magnesium base composite material bar of 5mm.
Claims (1)
1. a boron doped carbon nanotube strengthens method of preparing magnesium-based composite material, and its embodiment comprises following process:
1) with B
2O
3As the boron source, it is 10: 1 by the atomic ratio of boron atom and carbon atom, with B
2O
3Put into Noah's ark bottom, the coated carbon nanotube places tube furnace with Noah's ark more in the above, is warming up to 1100-1300 ℃ with the temperature rise rate of 10 ℃/min, and insulation is 3-5 hour under the atmosphere of argon gas;
2) adopt three-sulfopropyl tetradecyl diformazan trimethyl-glycine surface bi ion active agent that the boron doped carbon nanometer pipe is disperseed, the mass ratio of dispersion agent and boron doped carbon nanometer pipe is 1: 10, dispersion agent is dissolved in the 200-300ml Virahol under 60 ℃ of temperature, the boron doped carbon nanometer pipe was joined in the gained solution ultrasonic agitation 30 minutes, the mass ratio of pressing boron doped carbon nanometer pipe and magnesium is (0.1-1.5): (99.9-98.5), to cross 200 purpose magnesium powder again joins in the gained solution, mixed 20-40 minute, suction filtration then, dry down and grind evenly at temperature 50-80 ℃, obtain the composite powder of boron doped carbon nanometer pipe with magnesium;
3) with step 2) composite powder of gained suppressed under pressure 500-700MPa 2-3 minute, having obtained diameter is the block of the matrix material of 20mm, temperature rise rate with 10 ℃/min is warming up to 500-600 ℃, under the protective atmosphere of argon gas, carried out sintering 1-3 hour, then the block that obtains was carried out multiple pressure 2-3 minute under pressure 600-750MPa, temperature rise rate with 10 ℃/min is warming up to 550-650 ℃, reburns to tie 1-3 hour under the protective atmosphere of argon gas; The cooling room temperature obtains the boron doped carbon nanometer pipe and strengthens magnesium base composite material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014399A (en) * | 2012-12-31 | 2013-04-03 | 哈尔滨工业大学 | Preparation method of enhanced magnesium-based composite material of carbon nanotubes |
| CN105552385A (en) * | 2016-03-16 | 2016-05-04 | 湘潭大学 | Boron-doped carbon material and preparation method and application thereof |
| CN114664497A (en) * | 2022-04-14 | 2022-06-24 | 北京化工大学 | Modified silver nanowire dispersion liquid, preparation method thereof and preparation method of transparent conductive electrode |
-
2011
- 2011-08-03 CN CN 201110220133 patent/CN102268580A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《天津大学硕士学位论文》 20100601 侯珍 硼掺杂碳纳米管增强镁基复合材料的制备及力学性能 , * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014399A (en) * | 2012-12-31 | 2013-04-03 | 哈尔滨工业大学 | Preparation method of enhanced magnesium-based composite material of carbon nanotubes |
| CN103014399B (en) * | 2012-12-31 | 2014-07-30 | 哈尔滨工业大学 | Preparation method of enhanced magnesium-based composite material of carbon nanotubes |
| CN105552385A (en) * | 2016-03-16 | 2016-05-04 | 湘潭大学 | Boron-doped carbon material and preparation method and application thereof |
| CN105552385B (en) * | 2016-03-16 | 2018-05-25 | 湘潭大学 | Boron doping carbon material and its preparation method and application |
| CN114664497A (en) * | 2022-04-14 | 2022-06-24 | 北京化工大学 | Modified silver nanowire dispersion liquid, preparation method thereof and preparation method of transparent conductive electrode |
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Application publication date: 20111207 |