CN109338134A - A kind of preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites - Google Patents
A kind of preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites Download PDFInfo
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- CN109338134A CN109338134A CN201811047081.5A CN201811047081A CN109338134A CN 109338134 A CN109338134 A CN 109338134A CN 201811047081 A CN201811047081 A CN 201811047081A CN 109338134 A CN109338134 A CN 109338134A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
Abstract
The present invention relates to a kind of preparation methods of nickel-plating carbon nanotube reinforced aluminum matrix composites, and steps are as follows: (1) carbon pipe surface is roughened: carbon nanotube being added in NaOH solution, roughing in surface is carried out；(2) carbon nano tube surface is sensitized: the carbon nanotube after roughing in surface is added to SnCl2It is handled in the mixed solution of HCl, is washed carbon nanotube with deionized water after completion processing.(3) carbon nano tube surface activates: treated that carbon nanometer changes pipe is added to PbCl for surface sensitizing2With surface active is carried out in the mixed solution of HCl；(4) Ni is plated on carbon nanotube surface: surface is carried out Electroless Plating Ni into the carbon nanotube after crossing roughening, being sensitized and activate in the nitrate solution of Ni；(5) molding of the composite material of nickel-plating carbon nanotube enhancing.
Description
Technical field
The present invention relates to a kind of preparations that aluminum matrix composite mechanical property is promoted using cold pressing-sintering molding mode
Method belongs to field of powder metallurgy.
Background technique
In recent years, with the development of the modern industries such as Aeronautics and Astronautics, automobile manufacture and military project, metal-base composites
Since its excellent performance has welcome broad application prospect.Wherein, aluminum matrix composite is even more and is given priority to and studied, this
It is because aluminum matrix composite has property not available for many other materials, for example, good corrosion resistance, density are low, have
Machinability and heat-resisting quantity etc..But with the high speed development of modern industry, to the various aspects of performance of aluminum matrix composite
More stringent requirements are proposed.Therefore, used such as whisker, ceramic particle and fiber tradition when aluminum matrix composite is prepared to increase
Current demand is mutually no longer satisfied by force.Therefore, the comprehensive performance for how improving aluminum matrix composite becomes recent researches
Hot spot.
Since carbon nanotube is found since 1991, the favor of scientific researcher has just been received.This is because carbon nanotube
With lesser density, the chemical stability of superelevation and while there is very high mechanical property.Therefore, carbon nanotube is considered
It is the ideal reinforced phase for preparing aluminum matrix composite.Currently, preparing aluminum matrix composite main method has: powder metallurgic method melts
Melt casting, pressure permeation method and agitating friction weldering etc..Wherein, powder metallurgy due to easy to operate and sintering temperature it is low etc. excellent
Point is widely used in preparing carbon nanotube enhanced aluminium-based composite material.But carbon nanotube is prepared by powder metallurgy at present
Reinforced aluminum matrix composites still have two challenges: first is that since the van der waals force between carbon nanotube makes carbon nanometer
Pipe forms reunion in aluminum substrate；Second is that the nonwetting problem of carbon nanotube and aluminum substrate.Therefore, carbon nanotube is solved in aluminium base
Dispersion problem in body and improves the interfacial wettability between carbon nanotube and aluminium and establish stable carbon-aluminium interface there is weight
The meaning wanted.
Summary of the invention
It is main it is an object of the invention to propose a kind of preparation method of novel nickel-plating carbon nanotube reinforced aluminum matrix composites
If by carbon nano tube surface nickel-loaded nanoparticle so as to improve the nonwetting phenomenon between carbon nanotube and aluminum substrate, finally
Realize being obviously improved for aluminum matrix composite mechanical property.To achieve the above object, the present invention is subject to by the following technical programs
It realizes.
A kind of preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites, steps are as follows:
(1) carbon pipe surface is roughened: carbon nanotube being added in NaOH solution, roughing in surface is carried out；
(2) carbon nano tube surface is sensitized: the carbon nanotube after roughing in surface is added to SnCl2With the mixed solution of HCl
In handled, completion processing after carbon nanotube is washed with deionized water.
(3) carbon nano tube surface activates: treated that carbon nanometer changes pipe is added to PbCl for surface sensitizing2With the mixing of HCl
Surface active is carried out in solution；
(4) Ni is plated on carbon nanotube surface: carbon nanotube nitrate in Ni of the surface into after crossing roughening, be sensitized and activate is molten
Electroless Plating Ni is carried out in liquid；
(5) molding of the composite material of nickel-plating carbon nanotube enhancing: by nickel-plating carbon nanotube powder made from step (1)-(4)
The ratio at end and aluminium powder 1:100~300 in mass ratio is placed in stainless steel jar mill, and wherein ratio of grinding media to material is 1:10, and with argon gas
As protective gas, mixed-powder is subjected to ball milling；Mixed composite powder is first carried out to the cold moudling of 500-600Mpa,
Later in an argon atmosphere, temperature carries out the sintering of 1h under conditions of being 600-630 DEG C, then by obtained block materials 500
Hot extrusion is carried out under the conditions of~600 DEG C, obtains the composite material of nickel-plating carbon nanotube enhancing later.
(2) in, SnCl2With the mixed solution of HCl, SnCl2Concentration be 8-12g/L, the concentration of HCl is 35-45ml/L.
(3) in, PbCl2With the mixed solution of HCl, PbCl2Concentration be 0.8-1.2g/L, the concentration of HCl is 25-35ml/
L。
The present invention uses chemical method to carry out nickel plating in carbon nano tube surface first, so that carbon nano tube surface Load Balanced
Nano nickle granules；Secondly, mixing by speed change ball milling to nickel-plating carbon nanotube and aluminium powder, it had both been able to maintain carbon nanometer in this way
The quality of pipe can effectively solve the dispersion problem of carbon nanotube again；Block is prepared finally by the method for cold-rolled sintered-hot extrusion
Composite material.By the introducing of nickel, the nonwetting problem between carbon nanotube and aluminium not only can solve, but also can be to avoid
Excessive interfacial reaction occurs between carbon nanotube and aluminum substrate, realizes being obviously improved for aluminum matrix composite mechanical property.
Detailed description of the invention
Fig. 1 is the SEM figure of nickel-plating carbon nanotube made from Examples 1 and 2.Show that carbon pipe surface is dispersed with many in figure
Having a size of tens nanometers of nickel particle.
Fig. 2 (a) is the TEM figure of nickel-plating carbon nanotube made from Examples 1 and 2.From in the figure can more obviously from
To the nickel particle of load.
Fig. 2 (b) is the TEM figure of nickel-plating carbon nanotube made from Examples 1 and 2.Carbon nanotube as can be seen from the figure
Other than loading nickel particle, good structure that carbon nanotube is still kept.
Fig. 2 (c), (d), (e) are the EDAX results under the transmission of nickel-plating carbon nanotube made from Examples 1 and 2.From this
It can be seen that nickel element is uniformly distributed on the carbon nanotubes in figure, agglomeration is not occurred, meanwhile, exist in carbon nanotube
Part oxygen element.
Fig. 3 is the embodiment of the present invention 1, the load-deformation curve of fine aluminium made from composite material made from 2 and comparative example 1.
Specific embodiment
Illustrate the present invention below with reference to specific example, but is not intended to limit the present invention.
Embodiment 1
(1) 1g carbon nanotube is added in the NaOH solution that concentration is 200g/L, roughing in surface under conditions of 80 DEG C
20min；
(2) carbon nanotube after roughing in surface is added to SnCl2In the mixed solution of (10g/L) and HCl (40ml/L),
And 3min is handled under conditions of 30 DEG C, carbon nanotube is washed with deionized water after completion processing；
(3) treated that carbon nanometer changes pipe is added to PbCl for surface sensitizing2The mixed solution of (1g/L) and HCl (30ml/L)
Middle carry out surface active；
(4) carbon nanotube by surface after roughening, sensitization and activation carries out chemical plating in the nitrate solution of Ni
Ni, electrolyte is by NiSO4·6H2O(20g/L)、CuSO4·5H2O(1.2g/L)、C6H8O7(15g/L)、H3BO3(40g/L) and
NaH2PO2(40g/L) composition, carries out Electroless Plating Ni 1h. to carbon nano tube surface under conditions of 70 DEG C
It (5) is 20-30 μm by mass fraction 1% and partial size by nickel-plating carbon nanotube powder made from step (1)-(4)
15g aluminium powder is placed in the stainless steel jar mill of 250ml, and wherein ratio of grinding media to material is 1:10, and using argon gas as protective gas.It will mixing
Powder carries out the speed change ball milling of 200 turns of 6h and 400 turn of 2h respectively, it is therefore an objective to will increase under the premise of guaranteeing the quality of carbon nanotube
It is strong to be mutually sufficiently mixed with aluminium powder.Mixed composite powder is first cold-pressed 3min under the pressure of 600Mpa, later temperature
To carry out the sintering of 1h in 630 DEG C of ar gas environments, then obtained block materials are subjected to hot extrusion under the conditions of 550 DEG C, it
The rodlike composite material of nickel-plating carbon nanotube enhancing is obtained afterwards.
(6) tensile sample is prepared with rodlike composite material obtained, carries out tensile property test.
Stretching of the Ni-CNTs reinforced aluminum matrix composites prepared by this example under cold-rolled sintered-hot extrusion pressure condition is strong
Degree is 214.9MPa, elongation percentage 27.7%, as a result as shown in 1 curve of embodiment in Fig. 3.
Embodiment 2
(1) 1g carbon nanotube is added in the NaOH solution that concentration is 200g/L, roughing in surface under conditions of 80 DEG C
20min；
(2) carbon nanotube after roughing in surface is added to SnCl2In the mixed solution of (10g/L) and HCl (40ml/L),
And 3min is handled under conditions of 30 DEG C, carbon nanotube is washed with deionized water after completion processing；
(3) treated that carbon nanometer changes pipe is added to PbCl for surface sensitizing2The mixed solution of (1g/L) and HCl (30ml/L)
Middle carry out surface active；
(4) surface is subjected to chemical plating into the carbon nanotube after crossing roughening, being sensitized and activate in the nitrate solution of Ni
Ni, electrolyte is by NiSO4·6H2O(20g/L)、CuSO4·5H2O(1.2g/L)、C6H8O7(15g/L)、H3BO3(40g/L) and
NaH2PO2(40g/L) composition, carries out Electroless Plating Ni 1h. to carbon nano tube surface under conditions of 70 DEG C
It (5) is 20-30 μm by mass fraction 2% and partial size by nickel-plating carbon nanotube powder made from step (1)-(4)
15g aluminium powder is placed in the stainless steel jar mill of 250ml, and wherein ratio of grinding media to material is 1:10, and using argon gas as protective gas.It will mixing
Powder carries out the speed change ball milling of 200 turns of 6h and 400 turn of 2h respectively, it is therefore an objective to will increase under the premise of guaranteeing the quality of carbon nanotube
It is strong to be mutually sufficiently mixed with aluminium powder.Mixed composite powder is first cold-pressed 3min under the pressure of 600Mpa, later in argon
In compression ring border, temperature carries out the sintering of 1h under conditions of being 630 DEG C, then obtained block materials are carried out under the conditions of 550 DEG C
Hot extrusion obtains the rodlike composite material of nickel-plating carbon nanotube enhancing later.
(6) tensile sample is prepared with rodlike composite material obtained, carries out tensile property test.
Stretching of the Ni-CNTs reinforced aluminum matrix composites prepared by this example under cold-rolled sintered-hot extrusion pressure condition is strong
Degree is 275.3MPa, elongation percentage 20.1%, as a result as shown in 2 curve of embodiment in Fig. 3.
Comparative example 1
(1) the 15g aluminium powder that partial size is 20-30 μm is placed in the stainless steel jar mill of 250ml, wherein ratio of grinding media to material is 1:
10, and using argon gas as protective gas.Mixed-powder is carried out to the speed change ball milling of 200 turns of 6h and 400 turn of 2h respectively.After ball milling
Powder 3min is first cold-pressed under the pressure of 600Mpa, later in an argon atmosphere, temperature carries out 1h under conditions of being 630 DEG C
Sintering, then obtained block materials are subjected to hot extrusion under the conditions of 550 DEG C, the club-shaped material of fine aluminium is obtained later.
(6) tensile sample is prepared with club-shaped material obtained, carries out tensile property test.
Tensile strength of the fine aluminium prepared by this example under cold-rolled sintered-hot extrusion pressure condition is 126.9MPa, elongation percentage
It is 22.3%, as a result as shown in 1 curve of comparative example in Fig. 3.
Claims (3)
1. a kind of preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites, steps are as follows:
(1) carbon pipe surface is roughened: carbon nanotube being added in NaOH solution, roughing in surface is carried out；
(2) carbon nano tube surface is sensitized: the carbon nanotube after roughing in surface is added to SnCl2It is carried out in the mixed solution of HCl
Processing washes carbon nanotube with deionized water after completion processing.
(3) carbon nano tube surface activates: treated that carbon nanometer changes pipe is added to PbCl for surface sensitizing2In the mixed solution of HCl
Carry out surface active；
(4) Ni is plated on carbon nanotube surface: by surface into the carbon nanotube crossed after being roughened, be sensitized and activating in the nitrate solution of Ni
Carry out Electroless Plating Ni；
(5) nickel-plating carbon nanotube enhancing composite material molding: by nickel-plating carbon nanotube powder made from step (1)-(4) with
The ratio of aluminium powder 1:100~300 in mass ratio is placed in stainless steel jar mill, wherein ratio of grinding media to material be 1:10, and using argon gas as
Mixed-powder is carried out ball milling by protective gas；Mixed composite powder is first carried out to the cold moudling of 500-600Mpa, later
In an argon atmosphere, temperature carries out the sintering of 1h under conditions of being 600-630 DEG C, then by obtained block materials 500~600
Hot extrusion is carried out under the conditions of DEG C, obtains the composite material of nickel-plating carbon nanotube enhancing later.
2. preparation method according to claim 1, which is characterized in that (2) in, SnCl2With the mixed solution of HCl, SnCl2
Concentration be 8-12g/L, the concentration of HCl is 35-45ml/L.
3. preparation method according to claim 1, which is characterized in that (3) in, PbCl2With the mixed solution of HCl, PbCl2
Concentration be 0.8-1.2g/L, the concentration of HCl is 25-35ml/L.
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Cited By (5)
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| CN112008087A (en) * | 2020-08-30 | 2020-12-01 | 中南大学 | Method for improving comprehensive performance of carbon nano material reinforced nickel-based high-temperature alloy |
| CN112652425A (en) * | 2020-07-27 | 2021-04-13 | 邵峥业 | Preparation method of carbon nano tube composite transparent conductive film |
| CN114807656A (en) * | 2022-03-16 | 2022-07-29 | 郑州航空工业管理学院 | Preparation method of nanoscale carbon material reinforced metal matrix composite material and product thereof |
| CN114934242A (en) * | 2022-05-24 | 2022-08-23 | 日善电脑配件(嘉善)有限公司 | Aluminum-based composite material and processing method thereof |
| CN115505910A (en) * | 2022-10-25 | 2022-12-23 | 北京航空航天大学 | Magnetic metal @ SiC wave-absorbing powder and preparation method thereof |
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Application publication date: 20190215 |