CN105088110A - Preparation method for nickel-plated carbon nano tube reinforced aluminum matrix composites - Google Patents
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Abstract
The invention provides a preparation method for nickel-plated carbon nano tube reinforced aluminum matrix composites. The method includes the steps that 1, the outer portion of a carbon nano tube is plated with nickel, so that a nickel-coated carbon nano tube is obtained; 2, aluminum powder or aluminum alloy powder, the nickel-coated carbon nano tube and a process control agent are mixed for ball-milling, so that composite powder is obtained; 3, the composite powder is packaged in a metal cover and is rolled after temperature rises, so that a composite material blank is obtained; 4, the metal cover is stripped, burs are removed, and then the nickel-plated carbon nano tube reinforced aluminum matrix composites are obtained. The nickel-plated carbon nano tube is used for improving the interface of the aluminum matrix composites, a high-temperature interface reaction between the carbon nano tube and an aluminum matrix can be avoided, and meanwhile wettability between the carbon nano tube and the aluminum matrix can be improved. Moreover, the nickel layer on the surface of the carbon nano tube can react with the aluminum matrix to generate intermetallic compounds, the interface bonding strength between the carbon nano tube and an aluminum matrix is improved, and accordingly the mechanical properties of the composite materials are improved.
Description
Technical field
The invention belongs to metal composite field, specifically refer to a kind of preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites.
Background technology
Metal-base composites has the premium properties of traditional metal materials, can overcome the performance limitation of traditional metal materials after adding wild phase.The advantages such as aluminum matrix composite has quality light, and intensity is high, wear resistant corrosion resistant, and the good and thermal expansivity of electrical and thermal conductivity is low, are widely used in space flight and aviation, automobile making, the industrial circles such as electronic machine.How carbon nanotube, as the common wild phase of one of aluminum matrix composite, utilizes the high performance aluminum matrix composite of carbon nanotube to become the focus studied this year both at home and abroad.
The dispersiveness of carbon nanotube in aluminum substrate is one of important factor affecting composite property.Carbon nanotube enhanced aluminium-based composite material preparation method has hot spray process, stirring casting method and squeeze casting method etc.Wherein hot spray process is that the carbon nanotube particulate of fusing or semi-molten is directly formed dense coating at substrate deposition in the mode of high-velocity jet, but temperature is very high in the technique of this method, easily cause carbon nanotube surface carbonation, affect the premium properties of carbon nanotube.Stirring casting method is uniformly mixed carbon nanotube and liquid aluminium, whole mixture is finally made to solidify, though the method technique is simple, but the wettability of aluminium to carbon nanotube is very poor, after composite material solidification, carbon nanotube and aluminum substrate there will be obvious demixing phenomenon, have great impact to the mechanical property of matrix material.Squeeze casting method is the prefabricated component by first preparing, by in the aluminium liquid impregnated preform under melting, finally by compacting, this technique exists due to High Pressure Solidification and viscous deformation simultaneously, product is without defects such as shrinkage cavity and porosities, but this technique could not dispersing Nano carbon tubes effectively, causes it to have obvious agglomeration in the base, has a great impact the performance of matrix material.
Summary of the invention
The object of the invention is the preparation method that a kind of nickel-plating carbon nanotube reinforced aluminum matrix composites is provided according to above-mentioned deficiency, the method utilizes the problem mode of carbon nanotube nickel plating being solved to carbon nanotube dispersiveness and wettability in aluminum substrate, improves the performance of carbon nanotube enhanced aluminium-based composite material.
The present invention is achieved in the following ways: a kind of preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites, and its step comprises:
(1) by outer for carbon nanotube nickel plating, the carbon nanotube of nickel coated is obtained;
(2) the process control agent mixing and ball milling that the carbon nanotube being the nickel coated of the 0.5-4.0% of aluminium powder or Al alloy powder by aluminium powder or Al alloy powder, mass percent, mass percent are the 0.5-2.0% of aluminium powder or Al alloy powder, obtains composite granule;
(3) composite granule is encapsulated in metal capsule, is rolled after being warming up to 400-620 DEG C, obtain matrix material blank;
(4) stripping metal jacket again, obtains described nickel-plating carbon nanotube reinforced aluminum matrix composites after removing burr.
Preferably, nickel plating in described step (1) first carboxylic carbon nano-tube is put into nickel salt solution to soak absorbed Ni ion, then the nickel ion of absorption is reduced into nickel simple substance as forming core core, finally plating in chemical plating fluid, obtains the carbon nanotube of described nickel coated.
Preferably, the nickel salt solution of described absorbed Ni ion is the aqueous solution of single nickel salt or nickelous chloride, and concentration is 0.1-0.8mol/L, and the time of described immersion is 10min-30min.
Preferably, the described nickel ion by absorption is reduced into nickel simple substance is that described strong reductant is any one in POTASSIUM BOROHYDRIDE, sodium borohydride, and concentration is 0.4-4.0mol/L, and the time of described reduction is 20-30min with strong reductant reduction.
Preferably, it is carry out in chemical plating fluid that the described nickel ion by absorption is reduced into nickel simple substance, and described chemical plating fluid comprises complexing agent, buffer reagent, weak reductant and nickel salt; Described complexing agent is any one in Trisodium Citrate, EDETATE DISODIUM or trolamine, described buffer reagent is any one in sodium-acetate or ammonium chloride, described weak reductant is any one in formaldehyde, diethylstilbestrol acid, dimethylacetamide amino acid or inferior sodium phosphate, and described nickel salt is single nickel salt or nickelous chloride.The conventional formulation that this chemical plating fluid is known to the skilled person.
Preferably, described carboxylic carbon nano-tube is multi-walled carbon nano-tubes, and caliber is 0.4-150nm.
Preferably, the aluminium powder in described step (2) refers to pure aluminium powder, and Al alloy powder refers to aluminium-silicon system, aluminum-magnesium series, Solder for Al-Cu Joint Welding system, aluminium-zinc system or rare earth aluminium alloy powder, and the powder granule median size of aluminium powder or Al alloy powder is 50nm-100 μm.
Preferably, the process control agent in described step (2) is any one in stearic acid, lithium stearate, Zinic stearas, paraffin, methyl alcohol, ethanol, silicone oil, oleic acid, Mierocrystalline cellulose.
Preferably, the ball milling in described step (2) refers to planetary type ball-milling or stirring ball-milling, and ratio of grinding media to material is 10/1-40/1, and rotating speed is 100-500 rev/min, and Ball-milling Time is 4-8 hour.
Preferably, the metal capsule in described step (3) is in copper or iron pipe shape thin-wall section; The described 400-620 of being warming up to DEG C is first rolling again after preheating 0.5-6 hour at 400-620 DEG C, and rolling pressure is 100-700MPa, under the amount of rolling be 0.1mm-5cm.
Beneficial effect of the present invention is:
Present invention uses the interface of nickel-plating carbon nanotube to aluminum matrix composite to improve, relative to traditional carbon nanotube enhanced aluminium-based composite material, nickel-plating carbon nanotube can avoid the high-temperature interface between carbon nanotube and aluminum substrate to react, and can also improve the wettability between carbon nanotube and aluminum substrate simultaneously.Further, in nickel-plating carbon nanotube reinforced aluminum matrix composites preparation process, carbon nano tube surface nickel dam can react with aluminum substrate and generate intermetallic compound, improves the interface bond strength of carbon nanotube and aluminum substrate, thus improves composite materials property.Meanwhile, use nickel-plating carbon nanotube to combine with the hot rolling of powder spheroidal graphite technique, more effectively solve uniformly dispersed in aluminum substrate of carbon nanotube.Nickel plating mode technique of the present invention is simple in addition, and cost is low, is applicable to suitability for industrialized production, has very strong practicality.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the fracture apperance of embodiment 1 nickel-plating carbon nanotube reinforced aluminum matrix composites 1;
Fig. 2 is the electron scanning micrograph of nickel-plating carbon nanotube at incision position fracture pattern of embodiment 1 nickel-plating carbon nanotube reinforced aluminum matrix composites 1.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment and accompanying drawing:
Embodiment 1
A preparation method for nickel-plating carbon nanotube reinforced aluminum matrix composites, its step comprises:
(1) be that many walls carboxylic carbon nano-tube of 100nm puts into the NiSO that concentration is 0.2mol/L by caliber
4soak 10min in solution, allow the surface adsorption Ni of carboxylic carbon nano-tube
2+, by washed with de-ionized water after immersion; By surface adsorption Ni
2+carbon nanotube put into the KBH of 0.4mol/L
4in solution, under ultrasonic wave decentralized environment, reductase 12 0min, is reduced into nickel simple substance by the nickel ion of absorption, uses washed with de-ionized water subsequently; Carbon nanotube with nickel simple substance is put into containing NiSO
46H
2o25g/L, NaHPO
2h
2o20g/L, Na
2c
6h
5o
72H
2o20g/L, NaAc (anhydrous) 5g/L, pH are in the beaker of the 200ml of 6.0, and be placed in 80 DEG C of thermostatical oil baths, plating 30min obtains the carbon nanotube of nickel coated;
(2) be the pure aluminium powder 40g of 20 microns by median size, account for the carbon nanotube 0.8g that aluminium powder mass percent is the nickel coated of 2.0%, with account for aluminium powder mass percent be 0.5% process control agent stearic acid 0.2g three mix, adopt planetary type ball-milling technique, ratio of grinding media to material is 10/1, rotating speed is 300rpm/min, Ball-milling Time 8 hours, obtained composite granule;
(3) be encapsulated in by composite granule in copper pipe shape thin-walled material jacket, first preheating rolling again after 2 hours at 450 DEG C, rolling pressure is 300MPa, under the amount of rolling be 2cm, obtain matrix material blank;
(4) stripping metal jacket again, obtains described nickel-plating carbon nanotube reinforced aluminum matrix composites 1 after removing burr.
Embodiment 2
A preparation method for nickel-plating carbon nanotube reinforced aluminum matrix composites, its step comprises:
(1) be that many walls carboxylic carbon nano-tube of 80nm puts into the NiCl that concentration is 0.1mol/L by caliber
2soak 30min in solution, allow the surface adsorption Ni of carboxylic carbon nano-tube
2+, by washed with de-ionized water after immersion; By surface adsorption Ni
2+carbon nanotube put into the KBH of 4mol/L
4in solution, under ultrasonic wave decentralized environment, reductase 12 0min, is reduced into nickel simple substance by the nickel ion of absorption, uses washed with de-ionized water subsequently; Carbon nanotube with nickel simple substance is put into containing NiCl
26H
2o25g/L, NaHPO
2h
2o20g/L, Na
2c
6h
5o
72H
2o20g/L, NaAc (anhydrous) 5g/L, pH are in the beaker of the 200ml of 6.0, and be placed in 80 DEG C of thermostatical oil baths, plating 30min obtains the carbon nanotube of nickel coated;
(2) be the Solder for Al-Cu Joint Welding powder 40g of 20 microns by median size, account for the carbon nanotube 0.2g that aluminium powder mass percent is the nickel coated of 0.5%, with account for aluminium powder mass percent be 0.5% process control agent silicone oil 0.2g three mix, adopt planetary type ball-milling technique, ratio of grinding media to material is 20/1, rotating speed is 100rpm/min, Ball-milling Time 4 hours, obtained composite granule;
(3) be encapsulated in by composite granule in copper pipe shape thin-walled material jacket, first preheating rolling again after 6 hours at 400 DEG C, rolling pressure is 700MPa, under the amount of rolling be 5cm, obtain matrix material blank;
(4) stripping metal jacket again, obtains described nickel-plating carbon nanotube reinforced aluminum matrix composites 2 after removing burr.
Embodiment 3
A preparation method for nickel-plating carbon nanotube reinforced aluminum matrix composites, its step comprises:
(1) be that many walls carboxylic carbon nano-tube of 150nm puts into the NiSO that concentration is 0.8mol/L by caliber
4soak 20min in solution, allow the surface adsorption Ni of carboxylic carbon nano-tube
2+, by washed with de-ionized water after immersion; By surface adsorption Ni
2+carbon nanotube put into the KBH of 1mol/L
4in solution, under ultrasonic wave decentralized environment, reduction 15min, is reduced into nickel simple substance by the nickel ion of absorption, uses washed with de-ionized water subsequently; Carbon nanotube with nickel simple substance is put into containing NiSO
46H
2o25g/L, NaHPO
2h
2o20g/L, Na
2c
6h
5o
72H
2o20g/L, NaAc (anhydrous) 5g/L, pH are in the beaker of the 200ml of 6.0, and be placed in 80 DEG C of thermostatical oil baths, plating 30min obtains the carbon nanotube of nickel coated;
(2) by median size be 50 nanometers aluminium-iron powder 40g, account for the carbon nanotube 0.4g that aluminium-iron powder mass percent is the nickel coated of 1.0%, with account for aluminium powder mass percent be 0.5% process control agent paraffin 0.2g three mix, adopt planetary type ball-milling technique, ratio of grinding media to material is 30/1, rotating speed is 500rpm/min, Ball-milling Time 6 hours, obtained composite granule;
(3) be encapsulated in by composite granule in copper pipe shape thin-walled material jacket, first preheating rolling again after 2 hours at 450 DEG C, rolling pressure is 600MPa, under the amount of rolling be 1cm, obtain matrix material blank;
(4) stripping metal jacket again, obtains described nickel-plating carbon nanotube reinforced aluminum matrix composites 3 after removing burr.
Embodiment 4
A preparation method for nickel-plating carbon nanotube reinforced aluminum matrix composites, its step comprises:
(1) be that many walls carboxylic carbon nano-tube of 0.4nm puts into the NiSO that concentration is 0.5mol/L by caliber
4soak 20min in solution, allow the surface adsorption Ni of carboxylic carbon nano-tube
2+, by washed with de-ionized water after immersion; By surface adsorption Ni
2+carbon nanotube put into the NaBH of 2mol/L
4in solution, under ultrasonic wave decentralized environment, reduction 30min, is reduced into nickel simple substance by the nickel ion of absorption, uses washed with de-ionized water subsequently; Carbon nanotube with nickel simple substance is put into containing NiSO
46H
2o25g/L, NaHPO
2h
2o20g/L, Na
2c
6h
5o
72H
2o20g/L, NaAc (anhydrous) 5g/L, pH are in the beaker of the 200ml of 6.0, and be placed in 80 DEG C of thermostatical oil baths, plating 30min obtains the carbon nanotube of nickel coated;
(2) by median size be 100 nanometers aluminum-magnesium powder 40g, account for the carbon nanotube 0.6g that aluminum-magnesium powder mass percent is the nickel coated of 1.5%, with account for aluminum-magnesium powder mass percent be 1% process control agent methyl alcohol 0.4g three mix, adopt stirring ball-milling technique, ratio of grinding media to material is 40/1, rotating speed is 300rpm/min, Ball-milling Time 8 hours, obtained composite granule;
(3) be encapsulated in by composite granule in iron pipe shape thin-walled material jacket, first preheating rolling again after 0.5 hour at 620 DEG C, rolling pressure is 100MPa, under the amount of rolling be 1mm, obtain matrix material blank;
(4) stripping metal jacket again, obtains described nickel-plating carbon nanotube reinforced aluminum matrix composites 4 after removing burr.
Embodiment 5
A preparation method for nickel-plating carbon nanotube reinforced aluminum matrix composites, its step comprises:
(1) be that many walls carboxylic carbon nano-tube of 100nm puts into the NiSO that concentration is 0.6mol/L by caliber
4soak 10min in solution, allow the surface adsorption Ni of carboxylic carbon nano-tube
2+, by washed with de-ionized water after immersion; By surface adsorption Ni
2+carbon nanotube put into the KBH of 4mol/L
4in solution, under ultrasonic wave decentralized environment, reductase 12 0min, is reduced into nickel simple substance by the nickel ion of absorption, uses washed with de-ionized water subsequently; Carbon nanotube with nickel simple substance is put into containing NiSO
46H
2o25g/L, NaHPO
2h
2o20g/L, Na
2c
6h
5o
72H
2o20g/L, NaAc (anhydrous) 5g/L, pH are in the beaker of the 200ml of 6.0, and be placed in 80 DEG C of thermostatical oil baths, plating 30min obtains the carbon nanotube of nickel coated;
(2) be the aluminium-silica flour 40g of 100 microns by median size, account for the carbon nanotube 1.6g that aluminium-silica flour mass percent is the nickel coated of 4%, with account for aluminium-silica flour mass percent be 2% process control agent Mierocrystalline cellulose 0.8g three mix, adopt planetary type ball-milling technique, ratio of grinding media to material is 10/1, rotating speed is 300rpm/min, Ball-milling Time 4 hours, obtained composite granule;
(3) be encapsulated in by composite granule in aluminum pipe shape thin-walled material jacket, first preheating rolling again after 1 hour at 600 DEG C, rolling pressure is 100MPa, under the amount of rolling be 0.1mm, obtain matrix material blank;
(4) stripping metal jacket again, obtains described nickel-plating carbon nanotube reinforced aluminum matrix composites 5 after removing burr.
As Fig. 1-2 can find out, extract form by nickel-plating carbon nanotube at incision position, can find out nickel-plating carbon nanotube and aluminum substrate bonding strength good, in large multi-embedding aluminum substrate, that directly extracts is little, and form the effect of connection bridge between carbon nanotube and aluminum substrate, the performance contributing to matrix material improves.And matrix material is less at incision position torn grain, dimple is less.
Obtained by embodiment 1-5 nickel-plating carbon nanotube reinforced aluminum matrix composites 1-5 tensile strength of mechanical property and hardness as shown in table 1:
| Tensile strength Mpa | Hardness HBW | |
| Embodiment 1 | 297 | 90.12 |
| Embodiment 2 | 307 | 86.55 |
| Embodiment 3 | 321 | 89.36 |
| Embodiment 4 | 346 | 96.93 |
| Embodiment 5 | 265 | 86.38 |
Table 1 carbon nanotube enhanced aluminium-based composite material 1-5 tensile strength and hardness
Claims (10)
1. a preparation method for nickel-plating carbon nanotube reinforced aluminum matrix composites, its step comprises:
(1) by outer for carbon nanotube nickel plating, the carbon nanotube of nickel coated is obtained;
(2) the process control agent mixing and ball milling that the carbon nanotube being the nickel coated of the 0.5-4.0% of aluminium powder or Al alloy powder by aluminium powder or Al alloy powder, mass percent, mass percent are the 0.5-2.0% of aluminium powder or Al alloy powder, obtains composite granule;
(3) composite granule is encapsulated in metal capsule, is rolled after being warming up to 400-620 DEG C, obtain matrix material blank;
(4) stripping metal jacket again, obtains described nickel-plating carbon nanotube reinforced aluminum matrix composites after removing burr.
2. the preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites according to claim 1, it is characterized in that: the nickel plating in described step (1) first carboxylic carbon nano-tube is put into nickel salt solution to soak absorbed Ni ion, then the nickel ion of absorption is reduced into nickel simple substance as forming core core, last plating in chemical plating fluid, obtains the carbon nanotube of described nickel coated.
3. the preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites according to claim 2, it is characterized in that: the nickel salt solution of described absorbed Ni ion is the aqueous solution of single nickel salt or nickelous chloride, concentration is 0.1-0.8mol/L, and the time of described immersion is 10min-30min.
4. the preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites according to claim 2, it is characterized in that: it is reduce with strong reductant that the described nickel ion by absorption is reduced into nickel simple substance, described strong reductant is any one in POTASSIUM BOROHYDRIDE, sodium borohydride, concentration is 0.4-4.0mol/L, and the time of described reduction is 20-30min.
5. the preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites according to claim 2, it is characterized in that: it is carry out in chemical plating fluid that the described nickel ion by absorption is reduced into nickel simple substance, and described chemical plating fluid comprises complexing agent, buffer reagent, weak reductant and nickel salt; Described complexing agent is any one in Trisodium Citrate, EDETATE DISODIUM or trolamine, described buffer reagent is any one in sodium-acetate or ammonium chloride, described weak reductant is any one in formaldehyde, diethylstilbestrol acid, dimethylacetamide amino acid or inferior sodium phosphate, and described nickel salt is single nickel salt or nickelous chloride.
6. the preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites according to claim 2, it is characterized in that: described carboxylic carbon nano-tube is multi-walled carbon nano-tubes, caliber is 0.4-150nm.
7. the preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites according to claim 1, it is characterized in that: the aluminium powder in described step (2) refers to pure aluminium powder, Al alloy powder refers to aluminium-silicon system, aluminum-magnesium series, Solder for Al-Cu Joint Welding system, aluminium-zinc system or rare earth aluminium alloy powder, and the powder granule median size of aluminium powder or Al alloy powder is 50nm-100 μm.
8. the preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites according to claim 1, is characterized in that: the process control agent in described step (2) is any one in stearic acid, lithium stearate, Zinic stearas, paraffin, methyl alcohol, ethanol, silicone oil, oleic acid, Mierocrystalline cellulose.
9. the preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites according to claim 1, it is characterized in that: the ball milling in described step (2) refers to planetary type ball-milling or stirring ball-milling, ratio of grinding media to material is 10/1-40/1, rotating speed is 100-500 rev/min, and Ball-milling Time is 4-8 hour.
10. the preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites according to claim 1, is characterized in that: the metal capsule in described step (3) is copper or iron pipe shape thin-wall section; The described 400-620 of being warming up to DEG C is first rolling again after preheating 0.5-6 hour at 400-620 DEG C, and rolling pressure is 100-700MPa, under the amount of rolling be 0.1mm-5cm.
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| CN105200353A (en) * | 2015-10-17 | 2015-12-30 | 国家电网公司 | Preparation method of nickel-plated CNT (carbon nano tube) reinforced aluminum matrix composite |
| CN105778678A (en) * | 2016-04-22 | 2016-07-20 | 江苏联科纳米科技有限公司 | Water-based electrothermal coating and preparation method thereof |
| CN106513621A (en) * | 2016-11-21 | 2017-03-22 | 昆明理工大学 | Production method of graphene-aluminum composite |
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| CN110331311A (en) * | 2019-04-22 | 2019-10-15 | 江苏大学 | A kind of continuous preparation method of in-situ ceramic particle enhanced aluminum-based composite material |
| CN110951016A (en) * | 2019-12-13 | 2020-04-03 | 宁波丝路科技交流服务有限公司 | Preparation method of high-strength carbon nanotube/TiAl composite material |
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