CN104213057B - A kind of copper carbon fiber strengthens Al-Li Alloy Matrix Composites and preparation method thereof - Google Patents
A kind of copper carbon fiber strengthens Al-Li Alloy Matrix Composites and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of copper carbon fiber and strengthen Al-Li Alloy Matrix Composites and preparation method thereof.This matrix material is formed by copper carbon fiber and Al-Li alloy powder technique, copper carbon fiber volume fraction content 1 ~ 10%.Preparation method of the present invention mainly comprises the copper facing of carbon fiber, ball mill mixing and vacuum heating-press sintering.By regulating and controlling the volume fraction of copper carbon fiber, the density of Al-Li alloy can be reduced, promoting the intensity of Al-Li alloy, toughness improve its anisotropy, when mechanical property close to, alleviate more than 5% than conventional aluminium lithium alloy density.The present invention is specially adapted to require that material has the good aircraft component of lightweight, high strength, over-all properties.
Description
Technical field
The present invention relates to the preparation field of metal-base composites, a kind of copper carbon fiber strengthens Al-Li Alloy Matrix Composites and preparation method thereof specifically.
Background technology
Lithium is the metallic element that occurring in nature is the lightest, and density is only 0.534g/cm3, the density 1.732g/cm3 of magnesium, and the lithium often adding 1% (massfraction) in aluminium can make alloy density reduce by 3%, Young's modulus increase about 6%.
It is estimated that, compared with adopting the Boeing of conventional aluminum alloy manufacture, according to advanced Al-Li alloy for the manufacture of the fuselage weight by reduction by 14.6%, save the fuel consumption of 5.4%, reduce the manufacturing cost of 2.1%, every airplane is every year by the flight expense of reduction by 2.2%; Air fighter is also the key areas that Al-Li alloy takes the lead in launching application, if can alleviate the fuselage weight of 15%, will reduce by the aircraft ground run distance of 15%, extends the radius of 20%, increases by the useful load of 30% simultaneously.World-renowned flyer producer Airbus SAS has adopted a large amount of A1-Li alloy for the manufacture of A380 and A350, applies as floor bearer, fuselage skin and lower aerofoil stringer.
Research finds that A1-Li binary alloy exists that toughness is lower, anisotropy is serious, short transverse strength is lower, plasticity and toughness level is poor, can the problem such as heavy losses toughness after beat exposure, limit the application of Al-Li alloy in aircraft field.
In view of the over-all properties of A1-Li binary alloy is poor, usual needs on binary alloy basis separately or compound add the alloying elements such as Mg, Cu, Zr, Zn, Mn, Ag, thus form multiple strengthening phase, and change quantity and the distribution of strengthening phase, reach the object improving its performance, except document is reported for work, some are also had to application discloses the technological method improving Al-Li alloy performance.
Chinese patent application is found: " publication number CN103687971A; May 16 2012 applying date; patent name " has the magnalium lithium alloy of the fracture toughness property of improvement "; disclose and " prepared the Al-Li alloy containing lot of trace alloying element by molten-salt growth method, and improved the toughness of Al-Li alloy by follow-up hot-working process through technology retrieval.
Chinese patent application: " publication number CN103509984A; September 28 2013 applying date; patent name " a kind of Ultrahigh strength aluminum lithium alloy and preparation method thereof "; disclose " with the common combined microalloying strengthening of Mg, Ag, Zn trace element, prepare burden by alloying constituent, by melting sources, after furnace refining, leaving standstill, be cast into the alloy cast ingot of required specification, manufacture sheet material tensile strength and can reach more than 580MPa, unit elongation is higher than 7% simultaneously, can be used for the structural element in the fields such as aerospace, nuclear industry, communications and transportation, weapons ".
Chinese patent application: " publication number CN103255322A; June 2 2013 applying date, patent name " high tenacity ultrathin die-cast aluminum lithium alloy " discloses " having fatigue resistance, crack extension force, solidity to corrosion and thermotolerance all better Al-Li alloy by the content preparation controlling zinc, copper, manganese, lithium, strontium, lanthanum and cerium in alloy ".
Chinese patent application: " publication number CN102304653A; September 9 2011 applying date; patent name " magnalium lithium alloy of a kind of high-ductility two-phase yttrium-containing and preparation method thereof "; disclose " magnalium lithium alloy of a kind of high-ductility two-phase yttrium-containing and preparation method thereof, the concrete component of this alloy and by mass percentage and content as follows: Li9.50 ~ 10.80%, Al3.00 ~ 5.00%, Y0.50 ~ 0.70%, Zr0.10 ~ 0.30%, surplus is Mg ".
Chinese patent application: " publication number CN10201457A; October 27 2010 applying date; patent name " a kind of high-toughness aluminum lithium alloy and preparation method thereof " discloses " microstructure of the tough Al-Li alloy material of a kind of novel high-strength evenly, stable performance, be applicable to manufacture slab and squeeze wood ".
As can be seen from above-mentioned content of the patent, by adding trace alloying element and the performance such as toughness, intensity of Al-Li alloy can be significantly improved in conjunction with thermal treatment, hot-working process in Al-Li alloy.
Carbon fiber is a kind of thermotolerance, solidity to corrosion is good and density is lower, the functional fiber material that specific tenacity is higher.Carbon Fibre Reinforced Metal Matrix Composites not only has lower density, good intensity and wear resistance, and there is the features such as excellent conduction, thermal conductivity, fatigue resistance, electromagnetic wave shielding, thus it is widely used in the fields such as automobile, track traffic, aerospace.But research finds that the interface wetting property of carbon fiber and Al-Li alloy matrix is poor, therefore, in prior art, do not strengthen the precedent of Al-Li alloy matrix strength with carbon fiber.
Summary of the invention
For solving the problem of the interface wetting property difference of carbon fiber and Al-Li alloy matrix, the invention provides a kind of copper carbon fiber and strengthen Al-Li Alloy Matrix Composites and preparation method thereof, improve carbon fiber and Al-alloy based body interface wetting property, and inhibit surface reaction therebetween, thus make it possible to use carbon fiber to strengthen Al-Li alloy, to fall low-alloyed density, improve toughness and the anisotropy of alloy, improve the intensity of Al-Li alloy, expand the application space of Al-Li alloy.
The present invention is the technical scheme solving the problems of the technologies described above employing: a kind of copper carbon fiber strengthens Al-Li Alloy Matrix Composites, by particle diameter to be the Al-Li alloy powder of 10-15 micron and volume fraction thereof be 1 ~ 10% copper carbon fiber make, wherein, according to weight ratio, the moiety of Al-Li alloy powder be 1 ~ 2.5% Li, 0.1 ~ 3% Mg, Cu, the Mn of 0.1 ~ 0.5% of 1 ~ 2%, Zn and Al of Zr, 0.3-1.5% of 0.05 ~ 0.2% and inevitable impurity;
Described copper carbon fiber is obtained by the mode of electroless plating in the carbon fiber immersion plating solution of diameter 10 μm.
The pH value of described plating solution is 12-13, temperature is 40-50 DEG C, and the composition contained in plating solution is as follows: the yellow prussiate of potash of the sodium hydroxide of EDTA, 15-17g/L of the copper sulfate of 14-16g/L, the Seignette salt of 18-22g/L, 23-27g/L, the formaldehyde of 14-16ml/L, the second bipyridine of 5-7mg/L and 18-22mg/L.
Above-mentioned copper carbon fiber strengthens the preparation method of Al-Li Alloy Matrix Composites, comprises the following steps:
1) Copper Plating of Carbon Fiber
Secure ph is the plating solution of 12-13
Take that copper sulfate, Seignette salt, EDTA, sodium hydroxide, formaldehyde, second bipyridine and yellow prussiate of potash are soluble in water is mixed with plating solution respectively, in plating solution, the content of each composition is respectively: copper sulfate 14-16g/L, Seignette salt 18-22g/L, EDTA23-27g/L, sodium hydroxide 15-17g/L, formaldehyde 14-16ml/L, second bipyridine 5-7mg/L and yellow prussiate of potash 18-22mg/L, and the temperature limiting plating solution is 40-50 DEG C;
Carbon fiber be placed in the plating solution prepared and carry out electroless plating until the surface attachment of carbon fiber has polycrystalline copper coating under the state keeping stirring;
2) batch mixing
The copper-plated carbon fiber in surface in step 1) is joined in Al-Li alloy powder according to the ratio of volume fraction 1-10%, then adopts planetary ball mill batch mixing till not observing reunion, obtain raw material powder for subsequent use;
Wherein, the moiety of described Al-Li alloy powder be 1 ~ 2.5% Li, 0.1 ~ 3% Mg, Cu, the Mn of 0.1 ~ 0.5% of 1 ~ 2%, the Zn of Zr, 0.3-1.5% of 0.05 ~ 0.2%, all the other are Al and inevitable impurity;
3) alloy is fired
By step 2) in the raw material powder that obtains vacuum tightness be 0.001-0.005Pa, pressure sinters under being the condition of 30-100MPa, during sintering, with the temperature rise rate of per minute 30-80 DEG C temperature risen to 530-610 DEG C and keep this temperature 5-30min to complete sintering, naturally cooling to room temperature after having sintered and namely obtain product.
During described electroless plating, according to the corresponding proportional distribution plating solution of 2.5-3.5g carbon fiber of often liter of plating solution and the amount of carbon fiber.
The present invention's carbon fiber used have passed through following pre-treatment before copper facing: the carbon fiber choosing diameter 10 μm is cut into the short carbon fiber of 2-3mm, then by short carbon fiber calcination 10 ~ 60min at the temperature of 400 DEG C ~ 450 DEG C, treating it to be cooled to normal temperature, to be placed on mass concentration be boil 5-15min in the dilute nitric acid solution of 25%, be placed in the sodium hydroxide solution 2-10min that mass concentration is 15% after the short carbon fiber distilled water flushing filtered out again, again filter out the process that short carbon fiber distilled water repeatedly soaks and namely completes carbon fiber after rinsing;
Beneficial effect: the present invention is by the plated surface last layer polycrystalline copper coating at carbon fiber, thus improve the interface wetting property of carbon fiber and Al-Li alloy, also inhibits surface reaction therebetween simultaneously, and then make carbon fiber can be used to strengthen Al-Li alloy, reduce the density of alloy, improve toughness and the anisotropy of alloy, improve the intensity of Al-Li alloy, expand the application space of Al-Li alloy.After testing, product over-all properties of the present invention is good: density is at 2.40 ~ 2.65g/cm
3, tensile strength is between 530 ~ 595MPa, and hardness, between 90 ~ 115HV, some parts of aircraft has a good application prospect.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment 1
In the present embodiment, the moiety of Al-Li alloy powder used and weight percent are: the Li of 1%, the Mg of 3%, the Cu of 1%, Mn, the Zr of 0.05%, the Zn of 0.3% of 0.1%, copper carbon fiber volume content 1%, and all the other are Al and inevitable impurity.
Concrete preparation method is as follows:
(1) carbon fiber is put in plating solution, under electric stirring mode, carry out electroless plating.Solution composition is: copper sulfate 14g/L, Seignette salt 18g/L, EDTA23g/L, sodium hydroxide 15g/L, formaldehyde 14ml/L, second bipyridine 5mg/L, yellow prussiate of potash 18mg/L, and temperature is 40 DEG C, and pH value is 12, often liter of corresponding carbon fiber 3.5g of plating solution.After electroless plating terminates, copper plate well-crystallized, the polycrystalline Cu coating be made up of different orientation Cu crystal grain, thickness is about 1 μm;
(2) copper carbon fiber that step (1) is handled well is joined in Al-Li alloy powder by 1% volume fraction, adopt the abundant batch mixing of planetary ball mill 6 hours, till not observing reunion, the raw material mixed is loaded in dry glassware for subsequent use;
(3) powder mixed in step (2) is loaded in mould, the mould installing powdered alloy is put into sintering oven, when in vacuum oven, vacuum reaches 0.001Pa, sample to be exerted pressure the pressure of 30MPa, energising is with the ramp to 560 DEG C of per minute 30 DEG C, be incubated after 30 minutes and lower the temperature, be down to room temperature when temperature and take out sample.
Fibre reinforced Al-Li alloy powder property parameter prepared by the present embodiment is: density is 2.63g/cm
3, after ageing treatment, tensile strength reaches 538MPa, and hardness is 98HV, and fracture toughness property is 17.68MPam
1/2.
Embodiment 2
In the present embodiment, the moiety of Al-Li alloy powder used and weight percent are: the Li of 2%, the Mg of 0.1%, the Cu of 2%, Mn, the Zr of 0.2%, the Zn of 1.5% of 0.5%, copper carbon fiber volume content 10%, and all the other are Al and inevitable impurity.
Concrete preparation method is as follows:
(1) carbon fiber that pre-treatment is good is put in plating solution, under electric stirring mode, carry out electroless plating.Solution composition is: copper sulfate 16g/L, Seignette salt 22g/L, EDTA27g/L, sodium hydroxide 17g/L, formaldehyde 16ml/L, second bipyridine 7mg/L, yellow prussiate of potash 22mg/L, and temperature is 50 DEG C, and pH value is 13, often liter of corresponding carbon fiber 2.5g of plating solution.After electroless plating terminates, copper plate well-crystallized, the polycrystalline Cu coating be made up of different orientation Cu crystal grain, thickness is about 1 μm;
(2) the copper facing short carbon fiber that step (1) is handled well is joined in Al-Li alloy powder by 10% volume fraction, adopt the abundant batch mixing of planetary ball mill 8 hours, till not observing reunion, the raw material mixed is loaded in dry glassware for subsequent use;
(3) powder mixed in step (2) is loaded in mould, the mould installing powdered alloy is put into sintering oven, when in vacuum oven, vacuum reaches 0.005Pa, sample to be exerted pressure the pressure of 100MPa, energising is warming up to 610 DEG C with the temperature rise rate of per minute 80 DEG C, be incubated after 5 minutes and lower the temperature, be down to room temperature when temperature and take out sample.
Fibre reinforced Al-Li alloy powder property parameter prepared by the present embodiment is: density is 2.41g/cm
3, after ageing treatment, tensile strength reaches 545MPa, and hardness is 103HV, and fracture toughness property is 19.23MPam
1/2.
Embodiment 3
In the present embodiment, the moiety of Al-Li alloy powder used and weight percent are: the Li of 1.75%, the Mg of 1.55%, the Cu of 1.5%, Mn, the Zr of 0.1%, the Zn of 0.9% of 0.3%, copper carbon fiber volume content 5.5%, all the other are Al and inevitable impurity.
Concrete preparation method is as follows:
(1) carbon fiber that pre-treatment is good is put in plating solution, under electric stirring mode, carry out electroless plating.Solution composition is: copper sulfate 15g/L, Seignette salt 20g/L, EDTA25g/L, sodium hydroxide 16g/L, formaldehyde 15ml/L, second bipyridine 6mg/L, yellow prussiate of potash 20mg/L, and temperature is 45 DEG C, and pH value is 12.5, often liter of corresponding carbon fiber 3g of plating solution.After electroless plating terminates, copper plate well-crystallized, the polycrystalline Cu coating be made up of different orientation Cu crystal grain, thickness is about 1 μm;
(2) the copper facing short carbon fiber that step (1) is handled well is joined in Al-Li alloy powder by 5.5% volume fraction, adopt the abundant batch mixing of planetary ball mill 8 hours, till not observing reunion, the raw material mixed is loaded in dry glassware for subsequent use;
(3) powder mixed in step (2) is loaded in mould, the mould installing powdered alloy is put into sintering oven, when in vacuum oven, vacuum reaches 0.003Pa, sample to be exerted pressure the pressure of 65MPa, energising is warming up to 570 DEG C with the temperature rise rate of per minute 55 DEG C, be incubated after 17 minutes and lower the temperature, be down to room temperature when temperature and take out sample.
Fibre reinforced Al-Li alloy powder property parameter prepared by the present embodiment is: density is 2.52g/cm
3, after ageing treatment, tensile strength reaches 563MPa, and hardness is 101HV, and fracture toughness property is 18.51MPam
1/2.
Claims (2)
1. a copper carbon fiber strengthens Al-Li Alloy Matrix Composites, it is characterized in that: by particle diameter to be the Al-Li alloy powder of 10-15 μm and volume fraction thereof be 1 ~ 10% copper carbon fiber make, wherein, according to weight ratio, the moiety of Al-Li alloy powder be 1 ~ 2.5% Li, 0.1 ~ 3% Mg, Cu, the Mn of 0.1 ~ 0.5% of 1 ~ 2%, Zn and Al of Zr, 0.3-1.5% of 0.05 ~ 0.2% and inevitable impurity;
Described copper carbon fiber is obtained by the mode of electroless plating in the carbon fiber immersion plating solution of diameter 10 μm; The pH value of described plating solution is 12-13, temperature is 40-50 DEG C, and the composition contained in plating solution is as follows: the yellow prussiate of potash of the sodium hydroxide of EDTA, 15-17g/L of the copper sulfate of 14-16g/L, the Seignette salt of 18-22g/L, 23-27g/L, the formaldehyde of 14-16ml/L, the second bipyridine of 5-7mg/L and 18-22mg/L;
Above-mentioned copper carbon fiber strengthens the preparation method of Al-Li Alloy Matrix Composites, comprises the following steps:
1) Copper Plating of Carbon Fiber
Secure ph is the plating solution of 12-13
Take that copper sulfate, Seignette salt, EDTA, sodium hydroxide, formaldehyde, second bipyridine and yellow prussiate of potash are soluble in water is mixed with plating solution respectively, in plating solution, the content of each composition is respectively: copper sulfate 14-16g/L, Seignette salt 18-22g/L, EDTA23-27g/L, sodium hydroxide 15-17g/L, formaldehyde 14-16ml/L, second bipyridine 5-7mg/L and yellow prussiate of potash 18-22mg/L, and the temperature limiting plating solution is 40-50 DEG C;
Carbon fiber be placed in the plating solution prepared and carry out electroless plating until the surface attachment of carbon fiber has polycrystalline copper coating under the state keeping stirring;
2) batch mixing
The copper-plated carbon fiber in surface in step 1) is joined in Al-Li alloy powder according to the ratio of volume fraction 1-10%, then adopts planetary ball mill batch mixing till not observing reunion, obtain raw material powder for subsequent use;
Wherein, the moiety of described Al-Li alloy powder be 1 ~ 2.5% Li, 0.1 ~ 3% Mg, Cu, the Mn of 0.1 ~ 0.5% of 1 ~ 2%, the Zn of Zr, 0.3-1.5% of 0.05 ~ 0.2%, all the other are Al and inevitable impurity;
3) alloy is fired
By step 2) in the raw material powder that obtains vacuum tightness be 0.001-0.005Pa, pressure sinters under being the condition of 30-100MPa, during sintering, with the temperature rise rate of per minute 30-80 DEG C temperature risen to 530-610 DEG C and keep this temperature 5-30min to complete sintering, naturally cooling to room temperature after having sintered and namely obtain product.
2. copper carbon fiber according to claim 1 strengthens Al-Li Alloy Matrix Composites, it is characterized in that: during described electroless plating, according to the corresponding proportional distribution plating solution of 2.5-3.5g carbon fiber of often liter of plating solution and the amount of carbon fiber.
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| DE102015221078A1 (en) | 2015-10-28 | 2017-05-04 | Airbus Operations Gmbh | Fiber reinforced metal component for an aerospace vehicle and manufacturing process for fiber reinforced metal components |
| CN108203794B (en) * | 2018-01-04 | 2020-02-14 | 中南大学 | Short carbon fiber aluminum-based composite material and preparation method thereof |
| CN110343979B (en) * | 2019-08-30 | 2020-08-28 | 沈阳工业大学 | Preparation method of titanium coating reinforced aluminum matrix composite |
| CN115852275B (en) * | 2022-03-31 | 2024-01-09 | 南京航空航天大学 | Ultra-light high-strength fiber reinforced aluminum-lithium alloy composite material and preparation method thereof |
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| JPS5837141A (en) * | 1981-08-27 | 1983-03-04 | Sumitomo Chem Co Ltd | Production of fiber-reinforced composite metallic material |
| JPS60194039A (en) * | 1984-03-14 | 1985-10-02 | Toyota Central Res & Dev Lab Inc | Fiber-reinforced aluminum alloy composite material and its production |
| CN101967589B (en) * | 2010-10-27 | 2013-02-20 | 中国航空工业集团公司北京航空材料研究院 | Medium-strength high-toughness aluminum lithium alloy and preparation method thereof |
| CN101967588B (en) * | 2010-10-27 | 2012-08-29 | 中国航空工业集团公司北京航空材料研究院 | Damage-resistant aluminum-lithium alloy and preparation method thereof |
| CN103243280B (en) * | 2013-04-28 | 2015-03-04 | 河南科技大学 | Carbon fiber reinforced aluminum-based composite material and preparation method thereof |
| CN103509984A (en) * | 2013-09-28 | 2014-01-15 | 中南大学 | Ultrahigh strength aluminum lithium alloy and preparation method thereof |
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