CN107083549A - A kind of method that welding prepares carbon nano-tube reinforced metal-matrix composite material - Google Patents
A kind of method that welding prepares carbon nano-tube reinforced metal-matrix composite material Download PDFInfo
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- CN107083549A CN107083549A CN201710132820.XA CN201710132820A CN107083549A CN 107083549 A CN107083549 A CN 107083549A CN 201710132820 A CN201710132820 A CN 201710132820A CN 107083549 A CN107083549 A CN 107083549A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
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Abstract
The present invention relates to a kind of method that welding prepares carbon nano-tube reinforced metal-matrix composite material, belong to field of metal matrix composite.The present invention first takes CNT to be put into mixed acid and purified, CNT after purification is added into ultrasonic disperse in absolute ethyl alcohol, obtain carbon nano tube suspension, modified and surfactant is sequentially added into suspension, it is put into refrigerator and stands after ultrasonic disperse, centrifuge to obtain modified carbon nano-tube, it is base material to take copper coin, laser treatment is carried out after polishing, obtain the copper coin base material after laser treatment, modified carbon nano-tube is welded on copper coin base material, it can obtain carbon nano-tube reinforced metal-matrix composite material, the present invention is modified and handled to CNT and base material respectively, so that CNT is uniformly dispersed in substrate surface, use welding procedure, CNT is set preferably to be embedded in copper plate base body material, and it is well combined with basal body interface, the mechanical property of composite can be improved.
Description
Technical field
The present invention relates to a kind of method that welding prepares carbon nano-tube reinforced metal-matrix composite material, belong to metal-based compound
Material Field.
Background technology
Copper has higher electrical conductivity, and excellent heat conductivility, and preferably processing ductility are widely used in electrically
Electronic applications.With the continuous progress of science and technology, for method institute of traditional addition third phase metal as the performance for improving copper
The Cu alloy material of production far can not meet demand of the society for high performance material.Because copper addition element causes material
Expect heat conduction, declining to a great extent for conductive characteristic, so ensureing the good heat conductive of copper, improves material while conductive physical property
Wear-resisting, the exploration in terms of the mechanical property of tensile strength is particularly important.It is copper-based in order to prepare high performance carbon nanometer enhancing
Composite, researcher both domestic and external has done substantial amounts of research.It is dispersed in the base mainly around CNT, it is miscellaneous
Matter is few as much as possible, while keeping carbon nano tube structure integrality, matrix is well combined with carbon nanotube interface, it is ensured that composite wood
Studied in direction of the electrical conductivity of material more than 90%.
Carbon nanotube reinforced copper-base composite material traditional preparation methods are disadvantageous in that：（1）How CNT has
Effect be dispersed in metallic matrix for improve composite performance it is particularly significant, traditional preparation method for carbon nano-tube is generally adopted
It is that the method for mechanical agitation and ultrasonic cavitation is disperseed, but the CNT of this method is in the great molten metal of viscosity
Dispersion effect is unsatisfactory in body；（2）Traditional preparation method is related under high temperature, such as casting and powder metallurgic method, high temperature
What kind of reaction occurs between CNT meeting and metallic matrix, has no knowledge about at present, whether reactant can influence composite
Performance it is also indefinite；（3）It is that carbon is received that friction stir welding method, which prepares the maximum shortcoming of carbon nanotube reinforced copper-base composite material,
Mitron can not be evenly distributed in metallic matrix, even if reuniting forms graininess, but size and dispersed degree together
All not enough, the inhomogeneities of material property certainly will be caused；（4）CNT enhancing is prepared with chemical vapor deposition in-situ synthesis
Cu-base composites, although having obtained relatively good dispersion effect at present, need Ni as catalyst and preparation process ratio
More complicated, time-consuming.
The content of the invention
The present invention solves the technical problem of：Disperse uneven in metallic matrix for existing CNT, by
There is larger draw ratio in itself in CNT, specific surface area causes CNT easily to be reunited greatly, add metallic matrix material
In material, basal body interface combines the defect of difference there is provided a kind of method that welding prepares carbon nano-tube reinforced metal-matrix composite material,
The present invention first takes CNT to be put into mixed acid and purified, and CNT after purification is added into ultrasonic disperse in absolute ethyl alcohol,
Carbon nano tube suspension is obtained, is sequentially added into suspension and standing in refrigerator is put into after modified and surfactant, ultrasonic disperse,
Modified carbon nano-tube is centrifuged to obtain, it is base material to take copper coin, carries out laser treatment after polishing, obtains the copper coin base after laser treatment
Material, modified carbon nano-tube is welded on copper coin base material, you can obtain carbon nano-tube reinforced metal-matrix composite material, the present invention point
It is other that CNT and base material are modified and handled so that CNT is uniformly dispersed in substrate surface, use Welder
Skill, enables CNT to be preferably embedded in copper plate base body material, and is well combined with basal body interface, CNT pair
Cu-base composites have preferable enhancing effect, can improve the mechanical property of composite.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Weigh 4~6g CNTs, in mass ratio 1:5 add CNT in mixed acid, are taken out after 3~5h of stirring mixing
Filter, is obtained and is washed with deionized after filter residue 2~4 times, the filter residue after washing is put into baking oven, and 4 are dried at a temperature of 60~80 DEG C
~5h, obtains purifying carbon nano-tube；Described mixed acid is in mass ratio 2:1 by the nitric acid of mass fraction 65% and the sulphur of mass fraction 98%
Acid solution is mixed；
（2）Weigh the above-mentioned purifying carbon nano-tubes of 3~5g and be added to 150~170mL absolute ethyl alcohols, 10~15min of ultrasonic disperse is obtained
Carbon nano tube suspension, 1~3g cetyl trimethylammonium bromides and 2~4g 16 are sequentially added into carbon nano tube suspension
Sodium alkyl benzene sulfonate, continues 10~15min of ultrasonic disperse, and the mixed liquor after disperseing is placed in refrigerator, in -10~-5 DEG C of temperature
Take out, then be placed in baking oven after 5~7h of lower standing, standing, mixed liquor after 4~6h, standing is stood under the conditions of 100~120 DEG C
Add in centrifuge and centrifuge, obtain sediment, be put into baking oven, 8~10h is dried at a temperature of 40~50 DEG C, after drying
Modified carbon nano-tube, it is standby；
（3）It is that substrate is placed in polishing machine that to be polished to the roughness of copper coin substrate surface be 1.2~1.5 μm to take copper coin, will
Copper coin base material moves into C0 after polishing2It is 1500~2000W in laser power, spot size is 20mm × 1mm, is swept in laser
Speed is retouched to carry out being that can obtain surface to swash after 200~250ms of laser treatment, laser treatment under conditions of 120~140mm/min
Copper coin base material after light processing；
（4）By step（2）Standby modified carbon nano-tube is ultrasonically welded within the copper coin substrate surface after above-mentioned surface treatment, in frequency
Rate is that 25~30KHz, amplitude are 30~40 μm, under conditions of welding pressure is 18~20MPa, welds 150~200ms, welding
After be put into tube furnace, be warming up to 650~750 DEG C with 5~7 DEG C of heating rate, 2~3h of heat preservation sintering is cooled to after sintering
Room temperature is that can obtain standby carbon nano-tube reinforced metal-matrix composite material.
The application process of the present invention：The carbon nano-tube reinforced metal-matrix composite material that the present invention is prepared can exist extensively
Each type component of Aero-Space, automobile, the hardness that the present invention is prepared into composite is 58.5~60.2HV, than original copper
The hardness of plate base material 50~70%, maximum peeling force is 185.267~210.314N, and peeling force is more flat than original copper coin base material
32~40% are improved, tensile strength reaches 354~400MPa.
The beneficial effects of the invention are as follows：
（1）The present invention is modified and handled to CNT and base material respectively so that CNT uniformly disperses
In substrate surface, do not reunite；
（2）The present invention uses welding procedure, CNT is preferably embedded in copper plate base body material, and
And be well combined with basal body interface, CNT has preferable enhancing effect to Cu-base composites, can improve multiple
The mechanical property of condensation material.
Embodiment
Weigh 4~6g CNTs, in mass ratio 1:5 add CNT in mixed acid, are taken out after 3~5h of stirring mixing
Filter, is obtained and is washed with deionized after filter residue 2~4 times, the filter residue after washing is put into baking oven, and 4 are dried at a temperature of 60~80 DEG C
~5h, obtains purifying carbon nano-tube；Described mixed acid is in mass ratio 2:1 by the nitric acid of mass fraction 65% and the sulphur of mass fraction 98%
Acid solution is mixed；Weigh the above-mentioned purifying carbon nano-tubes of 3~5g and be added to 150~170mL absolute ethyl alcohols, ultrasonic disperse 10~
15min, obtains carbon nano tube suspension, and 1~3g cetyl trimethylammonium bromides and 2 are sequentially added into carbon nano tube suspension
~4g cetyl benzenesulfonic acid sodiums, continue 10~15min of ultrasonic disperse, and the mixed liquor after disperseing is placed in refrigerator, -10
Stand after 5~7h, standing and take out at a temperature of~-5 DEG C, then be placed in baking oven, 4~6h is stood under the conditions of 100~120 DEG C, it is quiet
Postpone mixed liquor and add centrifugation in centrifuge, obtain sediment, be put into baking oven, dry 8 at a temperature of 40~50 DEG C~
10h, obtains modified carbon nano-tube after drying, standby；Take copper coin to be placed in for substrate in polishing machine and be polished to copper coin substrate surface
Roughness be 1.2~1.5 μm, by after polishing copper coin base material move into C02 lasers in, laser power be 1500~2000W,
Spot size is 20mm × 1mm, and sweep speed is progress 200~250ms of laser treatment under conditions of 120~140mm/min, is swashed
The copper coin base material after surface laser processing is can obtain after light processing；Standby modified carbon nano-tube is ultrasonically welded within above-mentioned table
Copper coin substrate surface after the processing of face, frequency be 25~30KHz, amplitude be 30~40 μm, welding pressure be 18~20MPa's
Under the conditions of, 150~200ms is welded, is put into after welding in tube furnace, 650~750 DEG C is warming up to 5~7 DEG C of heating rate,
Room temperature is cooled to after 2~3h of heat preservation sintering, sintering and can obtain standby carbon nano-tube reinforced metal-matrix composite material.
Example 1
Weigh 4g CNTs, in mass ratio 1:5 add CNT in mixed acid, suction filtration after stirring mixing 3h, obtain filter residue
After be washed with deionized 2 times, the filter residue after washing is put into baking oven, at a temperature of 60 DEG C dry 4h, obtain purifying carbon nano-tube；
Described mixed acid is in mass ratio 2:1 is mixed by the nitric acid of mass fraction 65% and the sulfuric acid solution of mass fraction 98%；Weigh on 3g
State purifying carbon nano-tube and be added to 150mL absolute ethyl alcohols, ultrasonic disperse 10min obtains carbon nano tube suspension, it is outstanding to CNT
1g cetyl trimethylammonium bromides and 2g cetyl benzenesulfonic acid sodiums are sequentially added in supernatant liquid, continues ultrasonic disperse 10min, will
Mixed liquor after scattered is placed in refrigerator, is stood and is taken out after 5h, standing at a temperature of -10 DEG C, then is placed in baking oven, at 100 DEG C
Under the conditions of stand after 4h, standing mixed liquor and add in centrifuge and centrifuge, obtain sediment, be put into baking oven, in 40 DEG C of temperature
Lower dry 8h, obtains modified carbon nano-tube after drying, standby；Take copper coin to be placed in for substrate in polishing machine and be polished to copper coin base material
The roughness on surface is 1.2 μm, and copper coin base material after polishing is moved into C02It is 1500W, hot spot chi in laser power in laser
Very little is 20mm × 1mm, and sweep speed is i.e. available after laser treatment 200ms, laser treatment to be carried out under conditions of 120mm/min
Copper coin base material after surface laser processing；Standby modified carbon nano-tube is ultrasonically welded within to the copper coin base after above-mentioned surface treatment
Material surface, is that 25KHz, amplitude are 30 μm, under conditions of welding pressure is 18MPa in frequency, welds 150ms, be put into after welding
In tube furnace, 650 DEG C are warming up to 5 DEG C of heating rate, heat preservation sintering 2h is cooled to room temperature after sintering and can obtain standby carbon and receives
Mitron strengthens metal-base composites.
The carbon nano-tube reinforced metal-matrix composite material that the present invention is prepared can extensively Aero-Space, automobile it is each
Type component, the hardness that the present invention is prepared into composite is 58.5HV, maximum than the hardness 50% of original copper coin base material
Peeling force is 185.267N, and peeling force averagely improves 32% than original copper coin base material, and tensile strength reaches 354MPa.
Example 2
Weigh 5g CNTs, in mass ratio 1:5 add CNT in mixed acid, suction filtration after stirring mixing 4h, obtain filter residue
After be washed with deionized 3 times, the filter residue after washing is put into baking oven, at a temperature of 70 DEG C dry 4.5h, obtain purified carbon nanometer
Pipe；Described mixed acid is in mass ratio 2:1 is mixed by the nitric acid of mass fraction 65% and the sulfuric acid solution of mass fraction 98%；Weigh 4g
Above-mentioned purifying carbon nano-tube is added to 160mL absolute ethyl alcohols, and ultrasonic disperse 13min obtains carbon nano tube suspension, to CNT
2g cetyl trimethylammonium bromides and 3g cetyl benzenesulfonic acid sodiums are sequentially added in suspension, continues ultrasonic disperse 13min,
Mixed liquor after will be scattered is placed in refrigerator, is stood and is taken out after 6h, standing at a temperature of -8 DEG C, then is placed in baking oven, at 110 DEG C
Under the conditions of stand after 5h, standing mixed liquor and add in centrifuge and centrifuge, obtain sediment, be put into baking oven, in 45 DEG C of temperature
Lower dry 9h, obtains modified carbon nano-tube after drying, standby；Take copper coin to be placed in for substrate in polishing machine and be polished to copper coin base material
The roughness on surface is 1.3 μm, and copper coin base material after polishing is moved into C02 lasers, is 1700W, hot spot chi in laser power
Very little is 20mm × 1mm, and sweep speed is i.e. available after laser treatment 225ms, laser treatment to be carried out under conditions of 130mm/min
Copper coin base material after surface laser processing；Standby modified carbon nano-tube is ultrasonically welded within to the copper coin base after above-mentioned surface treatment
Material surface, is that 27KHz, amplitude are 38 μm, under conditions of welding pressure is 19MPa in frequency, welds 170ms, be put into after welding
In tube furnace, 700 DEG C are warming up to 6 DEG C of heating rate, heat preservation sintering 2.5h is cooled to room temperature after sintering and can obtain standby carbon
Nanotube strengthens metal-base composites.
The carbon nano-tube reinforced metal-matrix composite material that the present invention is prepared can extensively Aero-Space, automobile it is each
Type component, the hardness that the present invention is prepared into composite is 59.2HV, maximum than the hardness 60% of original copper coin base material
Peeling force is 195.512N, and peeling force averagely improves 38% than original copper coin base material, and tensile strength reaches 378MPa.
Example 3
Weigh 6g CNTs, in mass ratio 1:5 add CNT in mixed acid, suction filtration after stirring mixing 5h, obtain filter residue
After be washed with deionized 4 times, the filter residue after washing is put into baking oven, at a temperature of 80 DEG C dry 5h, obtain purifying carbon nano-tube；
Described mixed acid is in mass ratio 2:1 is mixed by the nitric acid of mass fraction 65% and the sulfuric acid solution of mass fraction 98%；Weigh on 5g
State purifying carbon nano-tube and be added to 170mL absolute ethyl alcohols, ultrasonic disperse 15min obtains carbon nano tube suspension, it is outstanding to CNT
3g cetyl trimethylammonium bromides and 4g cetyl benzenesulfonic acid sodiums are sequentially added in supernatant liquid, continues ultrasonic disperse 15min, will
Mixed liquor after scattered is placed in refrigerator, is stood and is taken out after 7h, standing at a temperature of -5 DEG C, then is placed in baking oven, in 120 DEG C of bars
Mixed liquor after 6h, standing is stood under part and adds centrifugation in centrifuge, sediment is obtained, is put into baking oven, at a temperature of 50 DEG C
10h is dried, modified carbon nano-tube is obtained after drying, it is standby；Take copper coin to be placed in for substrate in polishing machine and be polished to copper coin base material
The roughness on surface is 1.5 μm, and copper coin base material after polishing is moved into C02 lasers, is 2000W, hot spot chi in laser power
Very little is 20mm × 1mm, and sweep speed is i.e. available after laser treatment 250ms, laser treatment to be carried out under conditions of 140mm/min
Copper coin base material after surface laser processing；Standby modified carbon nano-tube is ultrasonically welded within to the copper coin base after above-mentioned surface treatment
Material surface, is that 30KHz, amplitude are 40 μm, under conditions of welding pressure is 20MPa in frequency, welds 200ms, be put into after welding
In tube furnace, 750 DEG C are warming up to 7 DEG C of heating rate, heat preservation sintering 3h is cooled to room temperature after sintering and can obtain standby carbon and receives
Mitron strengthens metal-base composites.
The carbon nano-tube reinforced metal-matrix composite material that the present invention is prepared can extensively Aero-Space, automobile it is each
Type component, the hardness that the present invention is prepared into composite is 60.2HV, maximum than the hardness 70% of original copper coin base material
Peeling force is 210.314N, and peeling force averagely improves 40% than original copper coin base material, and tensile strength reaches 400MPa.
Claims (1)
1. a kind of method that welding prepares carbon nano-tube reinforced metal-matrix composite material, it is characterised in that specifically preparation process is：
（1）Weigh 4~6g CNTs, in mass ratio 1:5 add CNT in mixed acid, are taken out after 3~5h of stirring mixing
Filter, is obtained and is washed with deionized after filter residue 2~4 times, the filter residue after washing is put into baking oven, and 4 are dried at a temperature of 60~80 DEG C
~5h, obtains purifying carbon nano-tube；Described mixed acid is in mass ratio 2:1 by the nitric acid of mass fraction 65% and the sulphur of mass fraction 98%
Acid solution is mixed；
（2）Weigh the above-mentioned purifying carbon nano-tubes of 3~5g and be added to 150~170mL absolute ethyl alcohols, 10~15min of ultrasonic disperse is obtained
Carbon nano tube suspension, 1~3g cetyl trimethylammonium bromides and 2~4g 16 are sequentially added into carbon nano tube suspension
Sodium alkyl benzene sulfonate, continues 10~15min of ultrasonic disperse, and the mixed liquor after disperseing is placed in refrigerator, in -10~-5 DEG C of temperature
Take out, then be placed in baking oven after 5~7h of lower standing, standing, mixed liquor after 4~6h, standing is stood under the conditions of 100~120 DEG C
Add in centrifuge and centrifuge, obtain sediment, be put into baking oven, 8~10h is dried at a temperature of 40~50 DEG C, after drying
Modified carbon nano-tube, it is standby；
（3）It is that substrate is placed in polishing machine that to be polished to the roughness of copper coin substrate surface be 1.2~1.5 μm to take copper coin, will
Copper coin base material moves into C0 after polishing2It is 1500~2000W in laser power, spot size is 20mm × 1mm, is swept in laser
Speed is retouched to carry out being that can obtain surface to swash after 200~250ms of laser treatment, laser treatment under conditions of 120~140mm/min
Copper coin base material after light processing；
（4）By step（2）Standby modified carbon nano-tube is ultrasonically welded within the copper coin substrate surface after above-mentioned surface treatment, in frequency
Rate is that 25~30KHz, amplitude are 30~40 μm, under conditions of welding pressure is 18~20MPa, welds 150~200ms, welding
After be put into tube furnace, be warming up to 650~750 DEG C with 5~7 DEG C of heating rate, 2~3h of heat preservation sintering is cooled to after sintering
Room temperature is that can obtain standby carbon nano-tube reinforced metal-matrix composite material.
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Cited By (1)
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| IT202200010511A1 (en) * | 2022-05-20 | 2023-11-20 | Istituto Naz Fisica Nucleare | METHOD OF PRODUCTION OF A MIXTURE OF PURE COPPER AND CARBON NANOTUBE AND OF ADDITIVE MANUFACTURING OF A NANOCOMPOSITE MATERIAL WITH A METALLIC MATRIX OF PURE COPPER REINFORCED WITH CARBON NANOTUBE BY MEANS OF SAID MIXTURE |
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