CN101817084A - Preparation method of micro-nano lamination metal base composite material - Google Patents
Preparation method of micro-nano lamination metal base composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of micro-nano lamination metal base composite material. Micro-nano flaky metal powder is added into solvent and then is prepared into flaky metal powder slurry, and the flaky metal powder slurry and nano reinforcement slurry are blended to ensure that the surface of the flaky metal powder evenly adsorbs the nano reinforcement and forms composite powder slurry; the metal powder slurry naturally stands to ensure that the flaky metal powder is parallel to the horizontal direction and subsides under the action of gravity, or an external force field is applied to accelerate flaky metal powder to be horizontally arranged and piled up; the solvent is removed to obtain lamination composite powder; and finally, the lamination composite powder is performed with densifying treatment to obtain compact micro-nano lamination metal base composite material. The method of the invention can prepare block micro-nano lamination metal base composite material, is environment-friendly, is simple, has high efficiency and is suitable for volume production.
Description
Technical field
That the present invention relates to is a kind of preparation method of technical field of composite materials, particularly be a kind of micro-nano lamination metal base composite material preparation method.
Background technology
Metal-base composites relies on its light in structure to quantize benefit and excellent wear-resisting, calorifics and electric property, realize business-like application at numerous areas such as automobile, electronics, space flight, aviation and Leisure Sport articles for use gradually, established status as new material and new technology.In traditional metal-base composites, pottery strengthens body and evenly distributes in metallic matrix, and along with the raising that strengthens the body volume fraction, the plasticity of metal-base composites and toughness all descend rapidly, are difficult to satisfy the engineering user demand.Therefore, emphasize gradually that in recent years artificial adjustment enhancing body presents orderly non-uniform Distribution on centre or meso-scale, so that further excavate the performance potential of metal-base composites, the optimization configuration of realization performance indications.Be subjected to Biocomposite materials such as nature bamboo and wood, shell, bone to reach inspiration strong, tough best fit with laminated construction, tough crisp lamination metal base composite material research more and more the causing concern that replaces, main purpose is the deficiency that compensates the monolayer material internal performance by ductile layers, to satisfy various special applications demands, for example exotic material, hardness material, heat barrier coat material etc.Result of study shows: the intensity of laminated material is 2 to 4 times of homogeneous material, and fracture toughness can reach more than 10 times of homogeneous material.The intensity of laminated material increases along with the minimizing of bilayer thickness (modulation wavelength), and reaches a peak value when being reduced to nanoscale.
Methods such as plasma spraying, magnetron sputtering, pulsed laser deposition, electro beam physics vapour deposition can prepare the film and the coating of nano-stack, but are difficult to the preparation block materials.Methods such as rolling diffusion, rolling formation, flow casting molding, injection forming can prepare the block laminated material, but are difficult to realize the nanometer bed thickness.Therefore, the method for seeking a kind of high-efficiency production of nano lamination block materials becomes the research focus in metal-base composites field.Powder metallurgy is metal-base composites preparation method commonly used, all adopts spherical or erose parent metal powder usually.Flaky metal powder has special two-dimension plane structure, have good adhesive force, covering power, albedo and excellent conducting performance, all be widely used in fields such as pigment, industrial coating, paint and printing ink, but the less preparation that is used for the Metal Substrate composite block material.
The oxide-dispersed alloy of present widespread usage, it is exactly in fact a kind of in-situ authigenic metal-base composite material, the crucial flaky metal powder that is to obtain high specific surface area of its preparation by wet ball grinding, thereby generate the oxide reinforcing particle by the surface oxidation original position, the shortcoming of this method is that the common content of generated in-situ enhancing body is lower, and be limited to oxide more, can't generate as even more ideal enhancing bodies such as CNT, carbon nano-fibers.On the other hand, can prepare flaky metal powder in advance, then the enhancing body blend that makes it and add by ball milling, external force such as mill.
Find through literature search prior art, people such as J.H.Lee roll up " the Characteristics of ceramic particlereinforced Al composite powder manufactured by a stone mill type crusher using twinroll cast Al alloy flake:a model on the formation of composite powder " that deliver on the 632nd page (adopt mill grinder mill double-roller rolling flaky aluminum alloyed powder and ceramic particle: the feature of composite powder and recombination process model) at " Materials Science andEngineering " calendar year 2001 A304-306, adding particle size in 5083 or 6061 flaky aluminum alloy powders of double-roller rolling is 1-3 μ m, and volume content is the Al of 10-20%
2O
3-TiC or Al
2O
3-B
4The C ceramic powders adopts the mill to death of burr grinder to form lamellar tissue.But the nanometer that this method is not suitable for as CNT, carbon nano-fiber strengthens body, because strengthening between the body, nanometer tends to reunite each other, only reliable long high-energy ball milling or mill could be realized evenly disperseing, so can seriously destroy the pattern of flaky metal powder and the structure that nanometer strengthens body, in fact can not obtain the nano-stack tissue.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of bulk metal based composites of micro-nano lamination is provided.It is raw material that the present invention adopts micro-nano flaky metal powder and nanometer to strengthen body, make nanometer strengthen body surperficial adsorbed by micro-nano flaky metal powder by the slip blend, utilize gravity then or add the orientation in the field of force, the promotion flaky metal powder is arranged in parallel and piles up, thereby forms the micro-nano lamination structure.
The present invention is achieved by the following technical solutions:
The present invention joins micro-nano flaky metal powder earlier and makes the flaky metal powder slip in the solvent, then flaky metal powder slip and nanometer are strengthened the blend of body slip, making the flaky metal powder surface evenly adsorb nanometer strengthens body and forms the composite powder slip, naturally leave standstill then flaky metal powder is arranged and sedimentation with horizontal direction parallel under the gravity effect, perhaps promote flaky metal powder to be to be arranged in parallel and pile up by applying external force field, remove solvent again and promptly obtain the lamination composite powder, after densification obtains closely knit lamination metal base composite material.
The present invention includes following steps:
(1) nanometer is strengthened body and join and stir in the solvent or ultrasonic dispersion, the preparation nanometer strengthens the body slip;
(2) micro-nano flaky metal powder is joined stir in the solvent or ultrasonic dispersion, preparation flaky metal powder slip;
(3) nanometer is strengthened body slip and flaky metal powder slip and mix, stir or ultrasonic dispersion strengthens body surperficial adsorbed by micro-nano flaky metal powder, formation composite powder slip until nanometer;
(4) stop to stir, utilize gravity or add the orientation in the field of force, promote micro-nano flaky metal powder in the composite powder slip to be arranged in parallel and pile up, remove solvent then, drying is handled and is promptly obtained the micro-nano lamination composite powder again;
(5) above micro-nano lamination composite powder is carried out densification, can obtain closely knit block micro-nano lamination metal base composite material.
Described micro-nano flaky metal powder is the one to multiple kind in aluminium, copper, magnesium, titanium and the alloy powder thereof, can adopt melt to get rid of any means preparations such as band, casting, ball milling, but must satisfy radius-thickness ratio greater than 10, thickness is between 200nm-5 μ m, and the sheet footpath is between 5-500um.
Described nanometer strengthens body size at least in one direction less than 100 nanometers, can be selected from the one to multiple kind in CNT, carbon nano-fiber, nano-carbide, nano-oxide, the nano nitride.
Described solvent can be selected from water or organic solvents such as methyl alcohol, ethanol, also can add function ingredients such as surfactant, defoamer in the slip.
Increase in body slip, micro-nano flaky metal powder slip and the composite powder slip in described nanometer, the shared volume ratio of solid phase is less than 20%.
The described field of force that adds is a kind of in centrifugal force field, field of pressure, the electromagnetic field.
In the described micro-nano lamination composite powder, the mass percent that nanometer strengthens body is 0.1-10%.
Described densification is earlier the micro-nano lamination composite powder to be cold-pressed into block, and then carries out thermal deformation processing such as hot pressing, high temperature insostatic pressing (HIP), hot extrusion, hot rolling.
It is raw material that the present invention adopts micro-nano flaky metal powder and nanometer to strengthen body, make nanometer strengthen body surperficial adsorbed by micro-nano flaky metal powder by the slip blend, " orientation " utilizing gravity simultaneously and add the field of force row that promotes to make even between the flaky metal powder is arranged spontaneous formation micro-nano lamination structure.As everyone knows, because two-dimension plane structure that flaky metal powder had, gravitate tends to be along the horizontal plane direction and is arranged in parallel in liquid, and the radius-thickness ratio of flakelike powder is big more, the shared volume ratio of liquid phase is big more in the slip, and this " horizontal orientation " effect is just obvious more.Therefore, the present invention requires the radius-thickness ratio of micro-nano flaky metal powder must be greater than 10, and the volume ratio in flaky metal powder slip and composite powder slip must be less than 20%.In addition, adding the field of force such as centrifugal force, gas pressure, electromagnetic force etc. can impel flaky metal powder to be equally to be arranged in parallel and pile up; If the direction of external force is consistent with gravity, then can strengthen " horizontal orientation " effect of gravity.In addition, removing solvent later stage or drying stage, the liquid film between the flakelike powder shrinks the pressure that is produced, and helps further to promote the parallel orientation in the laminated construction to arrange equally.
Metal dust is carried out wet ball grinding, can prepare flaky metal powder easily, and sheet footpath and thickness can be regulated and control in a big way, wherein thickness all is widely used in fields such as pigment, coating, paint and printing ink at the flaky metal powder of nanoscale, but the less preparation that is used for Metal Substrate block composite.The present invention at first adopts stirring or ultrasonic dispersion to prepare the flaky metal powder slip and nanometer strengthens the body slip, carries out the slip blend then, and in order to reduce maximum system energy, nanometer strengthens the surface that body tends to evenly be adsorbed in flaky metal powder.Slip blending technology of the present invention strengthens the destructive little of body to flaky metal powder and nanometer, form of the two and structure can intactly be remained, this helps to obtain the laminated construction of high-orientation, and regulate and control the thickness of lamellar structure easily by the thickness of flaky metal powder, wherein, nanometer strengthens body and is evenly distributed, and mass percent can regulation and control arbitrarily in the scope of 0.1%-10%.The present invention is simple, efficient, and green, environmental protection can prepare the bulk composite, are applicable to large-scale production.
Description of drawings
Fig. 1 operation principle schematic diagram of the present invention, the applied force field direction is parallel with gravity;
Fig. 2 operation principle schematic diagram of the present invention, the applied force field direction is vertical with gravity;
The electron microscope scanning photo of Fig. 3 micro-nano lamination composite powder of the present invention;
The electron microscope scanning photo of Fig. 4 micro-nano lamination composite of the present invention fracture.
The specific embodiment
Below in conjunction with accompanying drawing embodiment of the present invention is further described: following examples are being to implement under the prerequisite with the technical solution of the present invention; provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Carbon nano tube/copper nano-stack composite
Adopt the nano-sheet copper powder of ball milling preparation, sheet directly is about the 40-50 micron, the thick 300-400 nanometer that is about of sheet, and radius-thickness ratio is greater than 150; Employing contains the multi-walled carbon nano-tubes of carboxyl through strong acid treatment, surface, external diameter is the 20-60 nanometer.
CNT and surfactant lauryl sodium sulfate, defoamer octanol are added in the deionized water, ultrasonic dispersion made even carbon nanotube disperse in 2 hours, add deionized water then and regulate CNT concentration, obtaining concentration is the CNT slip of 5mg/ml;
Nano-sheet copper powder and surfactant polyethylene are joined in the absolute ethyl alcohol, and mechanical agitation is dissolved fully until polyethylene glycol, obtains solid volume content and be 10% nano-sheet copper powder slip;
The CNT slip is dropwise joined in the nano-sheet copper powder slip, carry out mechanical agitation simultaneously, make even carbon nanotube be adsorbed on the surface of nano-sheet copper powder, when the mass percent of CNT and nano-sheet copper powder reaches 0.5%, stop to drip and stirring;
Above gained carbon nano tube/copper composite powder slip is left standstill naturally, flake copper will be along the horizontal plane direction and be arranged in parallel, carry out vacuum filtration then and remove water and ethanol, in this process, composite powder sedimentation and pile up and be laminated construction under gravity and the effect of suction filtration pressure, its operation principle as shown in Figure 1, the applied force field direction is identical with gravity.The filter cake of above gained promptly obtains carbon nano tube/copper nano-stack composite powder again through 60 ℃ of vacuum drying 24 hours, and in dry run, the liquid film between the flakelike powder shrinks the pressure that is produced, and can further promote flakelike powder to align.With the microstructure of SEM sign gained nano-stack composite powder, as shown in Figure 3.
Earlier carbon nano tube/copper nano-stack composite powder is cold-pressed into base under 100 tons of pressure, hot pressed sintering 4 hours under 950 ℃ of argon gas atmosphere, 50 tons of pressure promptly obtains carbon nano tube/copper nano-stack composite then; With the fracture apperance of SEM sign gained nano-stack composite, as shown in Figure 4.
Embodiment 2
Boron carbide/aluminum micron laminated composite materials
Adopt the micron flake aluminum of ball milling preparation, its sheet directly is about the 50-70 micron, the thick 2-3 micron that is about of sheet, and radius-thickness ratio is greater than 25; Nanometer strengthens body and then adopts particle diameter to be about the nano silicon carbide boron particles of 50 nanometers.
Nano silicon carbide boron particles and surfactant neopelex are added in the deionized water, and ultrasonic dispersion made the nano boron carbide uniform particles disperse in 0.5 hour, obtained the nano boron carbide slip of solid volume content 5%;
Polyvinyl alcohol is added in the deionized water, be warming up to 95 ℃ after mechanical agitation dissolve fully until polyvinyl alcohol, obtain the polyvinyl alcohol water solution that concentration is 3wt%; The micron flake aluminum is joined in the polyvinyl alcohol water solution, and obtaining solid volume content through mechanical agitation is 20% micron flake aluminum slip;
A proper amount of nano boron carbide slip and a micron flake aluminum slip are mixed, and making the mass percent of wherein nano boron carbide and micron flake aluminum is 5%, and mechanical agitation is adsorbed on the surface of micron flake aluminum until the nano boron carbide uniform particles;
Above gained nano boron carbide/aluminium composite powder slip is placed filtering centrifuge, by the centrifugal action that is higher than 100 * g composite powder is piled up and be to remove moisture simultaneously by laminated construction; In this process, it is vertical with gravity to add the centrifugal force field direction, and its operation principle as shown in Figure 2.The filter cake of above gained promptly obtains nano boron carbide/aluminium micron lamination composite powder again through 60 ℃ of vacuum drying 24 hours; In dry run, the liquid film between the flakelike powder shrinks the pressure that is produced, and can further promote flakelike powder to align.
Nano boron carbide/aluminium micron lamination composite powder was removed organic matter in 2 hours in 300 ℃ of following heat treatments of argon gas atmosphere, again composite powder is cold-pressed into base under 100 tons of pressure, then 550 ℃ of following sintering of argon gas atmosphere 4 hours, under 450 ℃, carry out the vacuum hot extrusion at last, extrusion speed is 8mm/s, extrusion ratio is 20: 1, promptly obtains nano boron carbide/aluminium micron laminated composite materials.
Claims (10)
1. a micro-nano lamination metal base composite material preparation method is characterized in that, may further comprise the steps:
(1) nanometer is strengthened body and join and stir in the solvent or ultrasonic dispersion, the preparation nanometer strengthens the body slip;
(2) micro-nano flaky metal powder is joined stir in the solvent or ultrasonic dispersion, preparation flaky metal powder slip;
(3) nanometer is strengthened body slip and flaky metal powder slip and mix, stir or ultrasonic dispersion strengthens body surperficial adsorbed by micro-nano flaky metal powder, formation composite powder slip until nanometer;
(4) stop to stir, utilize gravity or add the orientation in the field of force, promote micro-nano flaky metal powder in the composite powder slip to be arranged in parallel and pile up, remove solvent then, drying is handled and is promptly obtained the micro-nano lamination composite powder again;
(5) above micro-nano lamination composite powder is carried out densification, can obtain closely knit block micro-nano lamination metal base composite material.
2. micro-nano lamination metal base composite material preparation method as claimed in claim 1 is characterized in that, described micro-nano flaky metal powder is the one to multiple kind in aluminium, copper, magnesium, titanium and the alloy powder thereof.
3. as claim 1 or 2 described micro-nano lamination metal base composite material preparation methods, it is characterized in that described micro-nano flaky metal powder radius-thickness ratio is greater than 10, thickness is between 200nm-5 μ m, and the sheet footpath is between 5-500um.
4. micro-nano lamination metal base composite material preparation method as claimed in claim 1 is characterized in that, described nanometer enhancing body is the one to multiple kind in CNT, carbon nano-fiber, nano-carbide, nano-oxide, the nano nitride.
5. as claim 1 or 4 described micro-nano lamination metal base composite material preparation methods, it is characterized in that described nanometer strengthens body size at least in one direction less than 100 nanometers.
6. micro-nano lamination metal base composite material preparation method as claimed in claim 1 is characterized in that, described solvent is water or methyl alcohol, ethanol.
7. micro-nano lamination metal base composite material preparation method as claimed in claim 1 is characterized in that, in described flaky metal powder slip and composite powder slip, the shared volume ratio of solid phase is less than 20%.
8. micro-nano lamination metal base composite material preparation method as claimed in claim 1 is characterized in that, the described field of force that adds is a kind of in centrifugal force field, field of pressure, the electromagnetic field.
9. micro-nano lamination metal base composite material preparation method as claimed in claim 1 is characterized in that, in the described micro-nano lamination composite powder, the mass percent that nanometer strengthens body is 0.1-10%.
10. micro-nano lamination metal base composite material preparation method as claimed in claim 1, it is characterized in that, described densification is earlier the micro-nano lamination composite powder to be cold-pressed into block, and then carries out thermal deformation processing such as hot pressing, high temperature insostatic pressing (HIP), hot extrusion, hot rolling.
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| CN113172228B (en) * | 2021-04-26 | 2022-05-13 | 中北大学 | TC (tungsten carbide)4-Al3Ti laminated composite board and preparation method thereof |
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