CN109929986A - A kind of composite material and preparation method - Google Patents
A kind of composite material and preparation method Download PDFInfo
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- CN109929986A CN109929986A CN201910176646.8A CN201910176646A CN109929986A CN 109929986 A CN109929986 A CN 109929986A CN 201910176646 A CN201910176646 A CN 201910176646A CN 109929986 A CN109929986 A CN 109929986A
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Abstract
The invention discloses a kind of composite materials, and boron nitride, silica, tungstic acid particle are evenly distributed in alloy matrix aluminum, and antifriction quality can be improved in molybdenum disulfide.The wearability and hardness that there are matrix surface three layers of gradient deposition layer can effectively improve alloy surface.The elements hardening constituent dispersion-strengtherning such as Zn, Sr, Ho, Cu, Au, Mg, Pd, Si, Al, Ni, W, Fe in alloy is to improve the mechanical property of material.Ceramic layer is formed by laser deposition in preparation method, promote primary alumina particle in sedimentary, it is rolled in conjunction with ultrasonic surface and further promotes hardness and wearability, combine ceramic high-temperature resistant after composite material surface ceramic, the low temperature resistant characteristic of metal makes that present invention could apply to need while high temperature resistant and low temperature resistant part manufacture field.Surface carburization technique can enhance the corrosion resistance of composite material.
Description
Technical field
The present invention relates to aluminum alloy materials field, in particular to a kind of composite material and preparation method.
Background technique
Currently, common aluminum alloy surface modification technology mainly has coating technology (plating, chemical plating, anodic oxygen both at home and abroad
Change), be vapor-deposited (PVD, CVD), plasma spray technology (electric arc spraying, flame-spraying, plasma spraying), high energy beam (laser, from
Beamlet, electron beam) a variety of methods such as process for modifying surface.Traditional aluminum alloy surface modification technology (coating technology, vapor deposition,
Plasma spray technology) though aluminum alloy hardness, wearability can be improved to a certain extent, but still there are some inevitable offices
It is sex-limited.As coating technology exists, obtained film plating layer is not fine and close enough, and chromate has toxicity, environmental pollution serious, three-protection design
Expense is high, endangers the deficiencies of human health place.PVD and CVD experiment condition are harsher, such as: coating is too thin, only micron
Grade；High temperature, high vacuum and high-purity material are needed, and with problem of environmental pollution.Hot-spraying coating institutional framework is stratiform knot
Structure, in coat inside, there are a large amount of holes and oxide to be mingled with.Cause coating's air hole ratio larger, bond strength is limited, often deposits
The problems such as cracking and flaking off.It cannot bear the mechanical working condition under high speed, top load.Laser surface treating technology is compared
Other conventional surface processing method advantages are: (1) being metallurgical bonding between coating and matrix；(2) strengthen thickness and densification, organize
It is tiny, hardness is high, wearability is good；(3) heat input is small, with short production cycle, and workpiece deformation is small；(4) non-environmental-pollution is that one kind is gathered around
Promising green manufacture technology.
Functionally gradient material (FGM) is a kind of completely new type heterogeneous material entirely different with homogeneous material, composite material, is mainly thought
Want for the different materials such as metal, ceramics, plastics to be combined with each other, forms the material with gradient function.Major way includes
The modified and whole layer structure two major classes in surface.The modified principle in surface is to utilize physics or change with metal or ceramics for matrix
Method forms single layer, multilayer or the continuous gradient structure with new capability.The central idea of whole layer structure be using by
Different kinds material is combined together by the method for layer distribution, forms the new material with multiple functions.
Glow discharge nitriding is one of most common active surface method for curing, and this thermo-chemical treatment can improve surface hardness
With contact durability wearability, this method obtains huge success in terms of modifying surface of ferrous material.But it is closed in aluminium
Use on gold also still rests on laboratory stage, can not carry out industrial volume production.The reason is as follows that described: (1) aluminium alloy seeps
What nitrogen process relied on is the combination of A1 atom He activity N atom, but solid solubility of the N atom in A1 lattice is very low, is difficult shape
At effective nitriding layer；(2) aluminum alloy surface easily forms one layer of naturally fine and close protective film, this layer of protective film hinders N original
The entrance of son；(3) resistance for the A1N that glow discharge nitriding is formed is very big, nitriding process glow discharge, and with nitriding process into
A1N layers of the row guiding discharge electric current that can thicken are too small, this will affect discharge process, also result in being hardly formed one layer of thicker infiltration
Nitrogen layer；(4) solid solubility temperature of general aluminium alloy is lower, this causes glow discharge nitriding temperature excessively high, reduces N atom active,
It is unfavorable for the formation of A1N.
CN104109782A provides a kind of aluminum alloy materials, aluminum alloy wear resistant member and preparation method thereof.The aluminium alloy material
Material includes weight percentage: 8~13% silicon, 1~2% zinc, the iron lower than 0.9%, is lower than 1~3% copper
0.9% manganese, the magnesium lower than 0.3% and the nickel lower than 0.5%, remaining is aluminium.Aluminum alloy materials with above-mentioned composition improve
Using it as the mechanical strength of workpiece obtained by raw material, and improve the wearability and processing characteristics of workpiece；And in aluminum alloy materials
The higher intensity that can further increase workpiece of Zn content, and then be effectively reduced the coefficient of friction of workpiece, improve workpiece
Wearability；Meanwhile content of magnesium control 0.3% hereinafter, can effectively prevent workpiece generate brittlement phase, reduce the extension of workpiece
Property, improve the wearability of workpiece, extend workpiece uses the time.
Foregoing invention only passes through the wearability for changing the component raising aluminium alloy of aluminum alloy materials, although can be to a certain degree
The wearability of upper enhancing aluminium alloy, but requirement that is limited, and being unable to satisfy while being under two kinds of extreme environments is acted on,
Such as the rigors of aluminum alloy materials in aero-engine, and it cannot be considered in terms of the corrosion resistance of material, use for a long time can be because of ring
The mechanical strength and mechanical properties decrease of material are corroded and caused in border, influences the application of material.
Summary of the invention
The technical problems to be solved by the invention: for present in aluminum current alloy-based wear-resistant material and its preparation process
Defect and deficiency, the present invention provide a kind of composite material, which has good wearability, hardness and corrosion resistance.
In order to solve the above technical problems, the present invention provides technical solution below:
A kind of composite material is evenly distributed with boron nitride, silica, tungstic acid, curing in the matrix of aluminium alloy
Molybdenum compound particles, aluminium alloy matrix surface have three layers of continuous gradient deposition layer, and three layers of gradient deposition layer are closed by laser in aluminium
Layer by layer deposition aluminium alloy/ceramic powder preparation on auri body, is followed successively by the first sedimentary, second according to deposition sequencing
Sedimentary, third sedimentary, aluminium alloy/ceramic powder are made pottery by 80~95wt% alloy matrix aluminum powder and 5~20wt%
Ceramic material powder constituent, the ceramic material is by 25~33wt% silicon carbide, 15~25wt% diboron trioxide, 25~35wt%
Titanium boride, 15~20wt% silica, 1~5wt% calcium oxide composition；The third deposition layer surface has nitriding layer；
The matrix composition of the aluminium alloy is according to weight percentage are as follows: 0.1-0.5%Cu, 0.004-0.006%Au,
0.8-1.2%Mg, 0.04-0.07%Pd, 0.05-0.08%Ni, 0.2-0.6%Zn, 0.2-0.4%Sr, 0.02-0.08%
Ho, 3-8%Si, 0.04-0.07%Fe, 0.002-0.008%W, surplus Al.
Preferably, boron nitride in the compound particles, silica, tungstic acid, molybdenum disulfide relative weight ratio be
1.1-1.4:1:1:0.03 weight percent of the compound particles in alloy matrix aluminum is 3-5%, the grain of compound particles
Diameter is 10-13 microns.
Preferably, aluminium alloy/ceramic powder ingredient that first sedimentary uses is 95wt% alloy matrix aluminum
Powder and 5wt% ceramic powder；The aluminium alloy that second sedimentary uses/ceramic powder ingredient is 88wt%
Alloy matrix aluminum powder and 12wt% ceramic powder；Aluminium alloy/ceramic powder that the third sedimentary uses at
It is divided into 80wt% alloy matrix aluminum powder and 20wt% ceramic powder.
Preferably, the average grain diameter of the aluminium alloy/ceramic powder is 0.1~1mm, the thickness of the gradient deposition layer
Degree is 4~6mm, the alloy matrix aluminum with a thickness of 20~40mm, the nitrided case depth is 60~150 μm.
A kind of preparation method of above-mentioned composite material includes following specific steps:
(1) alloy matrix aluminum being put into melting in electrical crucible, smelting temperature is 810~830 DEG C, 50-70 points of heat preservation
Master alloy liquid is obtained after clock, for use；Then it weighs and boron nitride, silica, tungstic acid, molybdenum disulfide is taken to be uniformly mixed preparation and mix
It is spare to close object powder；
(2) taking diameter is 6~8 millimeters of pure aluminum metal silk, and the length of silk is higher by 50~60 millimeters than type chamber height, will be golden
The half length for belonging to silk dips in epoxy resin liquid, and uniformly sprinkles mixture powder on it, after suspension stands 4~6 hours, with not
It dips in one end insertion clay sand mold cavity bottom molding sand of epoxy resin liquid, the depth being inserted into molding sand is 50~60mm, pure
The top and type chamber top surface of aluminum metal silk maintain an equal level；
(3) it can be poured at this time with mould assembling, the pouring temperature of alloy is 680~710 DEG C, the fine aluminium matched in master alloy liquid
Weight, needs to get rid of the weight of pure aluminum metal silk, 780 DEG C of 20~40min of heat preservation, make the evenly dispersed entrance of mixture powder after casting
In master alloy liquid, after natural cooling, casting is taken out, casting is cut into the plate of 20~40mm of thickness；
(4) prewired aluminium alloy/ceramic powder is sent to plate upper surface as current-carrying gas using argon gas and is deposited
Region, powder pushing precision reach 0.1g/min, then strike off powder, and layer thickness is 5~7mm；
(5) deposition region is strafed using optical fiber laser, 1.6~3.8KW of laser power, lasing beam diameter is 20~
40mm, 5~9mm/s of scanning speed, positioning accuracy reach 0.1mm, and machining area fills argon gas to 0.1~0.5MPa progress inertia
Gas shield, water oxygen content are brought down below 100ppm, and blowing argon gas is cooled to room temperature to form the first sedimentary after laser deposition processing；
(6) step (4) and (5) are repeated in the first sedimentary, form the second sedimentary, continue weight in the second sedimentary
Multiple step (4) and (5) form third sedimentary；
(7) by the plate solid solution aging containing three layers of gradient deposition layer: temperature is that 480~500 DEG C of solid solution 60mim exist later
It is cooling in normal-temperature water, then in 120~180 DEG C of 12~48h of timeliness, it is again heated in 490 DEG C of temperature the 20~30h that homogenizes, is taken
Room temperature is air-cooled to after out；
(8) plate through polishing polishing after, using ultrasonic surface rolling device carry out making Nano surface, supersonic frequency 25~
Amplitude is 30 μm, load 300N when 40kHz is processed, and lathe revolving speed is 200r/min, feed speed 0.07mm/rev, is surpassed
The hard alloy steel pellet impact 2.1~3.5 × 10 that every square millimeter of sample is 10mm by diameter after the completion of sound surface rolling4It is secondary；
(9) plate is put into chamber and is evacuated to 0.5~1 × 10-4, chamber is closed, chamber leak rate≤8Pa/ is measured
h；It is passed through ammonia, third is rinsed with 3~8w%NaOH and deposits layer surface, after 45min, extracts the ammonia in furnace out, and inject high-purity
It is started to warm up after nitrogen to 500~700Pa, when sample surface temperature reaches 560~640 DEG C, 6~9h of nitriding；
(10) cooled to room temperature takes out plate, heating plate to 300~400 DEG C of solid solution 1.5h, water cooling；It is heated to
100~110 DEG C of 50~100h of timeliness.
Preferably, the clay sand mold is prepared by water, kaolin and zircon sand, and zircon sand partial size is 60-80 mesh, kaolin
For the 9-13wt% of zircon sand, kaolin and zircon sand are put into after sand mixer after dry-mixed 10-15min, are added in sand mixer
The water of zircon sand 9-11wt% after continuing mixed grind 20-25 minutes, takes out moulding, shape forming cavity, sand mold bottom 65~75mm of thickness.
Preferably, the current-carrying gas pressure is 0.2MPa, carrier flow 2.2L/min, powder feed rate 2g/min.
It is that the present invention obtains the utility model has the advantages that
(1) boron nitride, silica, the hardness of tungstic acid are high, significantly improve the hardness and wearability of material, molybdenum disulfide
Antifriction quality can be improved.By adhering to boron nitride, silica, tungstic acid, molybdenum disulfide compound particles on pure aluminum metal silk
Mode be conducive to the quick of micro powder granule and spread and homogeneous so that mixed-powder is located at master alloy liquid center when casting, without
Melt back homogenizing, improves production efficiency.
(2) in alloy matrix aluminum, it can be achieved that refined crystalline strengthening, i.e., Zn, Sr, Ho improve the wetabilitys of aluminium alloy and foreign particles
The intensity of metal is improved by the refinement of crystallite size.Under external force, the dislocation pile up on crystal boundary generates a stress
, it can be used as the driving force that dislocation source is started in activation neighboring die.Cu, Au, Mg, Pd, Si, Al can realize solution strengthening,
Alloying element is solid-solution in parent metal the phenomenon that causing a degree of distortion of lattice to make alloy strength improve.Ni, W,
Fe can form dystectic compound, and Dispersed precipitate is in the base.The essence of hardening constituent dispersion-strengtherning is to utilize the super of disperse
Fine particles hinder the movement of dislocation, to improve the mechanical property of material.
(3) three layers of gradient deposition layer are formed by laser deposition aluminium alloy/ceramic powder, effectively by ceramic material
It combines closely with aluminum alloy materials, sedimentary is fine and close and is tightly combined between layers, can be significant after composite deposition ceramic material
The wearability and corrosion resistance of aluminum alloy base material are promoted, the high temperature of laser deposition can also promote primary aluminium oxide granule in sedimentary
Grain further promotes hardness and wearability, combines ceramic high-temperature resistant after composite material surface ceramic, metal is low temperature resistant
Characteristic makes that present invention could apply to need while high temperature resistant and low temperature resistant part manufacture field.
(4) surface carburization technique can further protect composite material surface, enhance the corrosion resistance of composite material, improve
Material uses the time.Ultrasonic surface rolling is carried out to gradient deposition layer by nano surface technique, further strengthens composite wood
Expect the hardness and wearability on surface.
Specific embodiment
Below by the description to embodiment, specific embodiments of the present invention will be described in further detail, with side
Those skilled in the art is helped to have more complete, accurate and deep understanding to inventive concept of the invention, technical solution.
Embodiment 1: it is prepared as follows composite material:
One, the preparation of raw material:
Aluminium alloy/ceramic powder is by 80~95wt% alloy matrix aluminum powder and 5~20wt% ceramic powder
Composition, the ceramic material is by 29wt% silicon carbide, 15wt% diboron trioxide, 35wt% titanium boride, 20wt% silica,
1wt% calcium oxide composition；
The matrix composition of aluminium alloy is according to weight percentage are as follows: 0.1%Cu, 0.004%Au, 0.8%Mg, 0.04%
Pd, 0.05%Ni, 0.2%Zn, 0.2%Sr, 0.02%Ho, 3%Si, 0.04%Fe, 0.002%W, surplus Al.
Boron nitride in compound particles, silica, tungstic acid, molybdenum disulfide relative weight ratio be 1.1:1:1:
0.03, weight percent of the compound particles in alloy matrix aluminum is 3%, and the partial size of compound particles is 10 microns.
The aluminium alloy that first sedimentary uses/ceramic powder ingredient is 95wt% alloy matrix aluminum powder and 5wt%
Ceramic powder；The aluminium alloy that second sedimentary uses/ceramic powder ingredient for 88wt% alloy matrix aluminum powder and
12wt% ceramic powder；The aluminium alloy that third sedimentary uses/ceramic powder ingredient is 80wt% alloy matrix aluminum
Powder and 20wt% ceramic powder successively increase the ratio of ceramic material in the powder, so that combining between deposition of layers
Closely, using transient mode but also the combination between matrix and sedimentary more closely, is not easy stress removing.Aluminium alloy/pottery
The average grain diameter of ceramic material powder is 0.1mm.
Two, the preparation of composite material
(1) alloy matrix aluminum is put into melting in electrical crucible, smelting temperature is 810 DEG C, and heat preservation obtains after 50 minutes
Master alloy liquid, for use；Then weigh take boron nitride, silica, tungstic acid, molybdenum disulfide to be uniformly mixed to prepare mixture powder standby
With；
(2) clay sand mold is prepared by water, kaolin and zircon sand, and zircon sand partial size is 60 mesh, and kaolin is zircon sand
Kaolin and zircon sand are put into after sand mixer after dry-mixed 10min, the water of zircon sand 9wt% are added in sand mixer by 9wt%,
Continue mixed grind after twenty minutes, takes out moulding, shape forming cavity, sand mold bottom thickness 65mm.
(3) taking diameter is 6 millimeters of pure aluminum metal silk, and the length of silk is higher by 50 millimeters than type chamber height, by wire
Half length dips in epoxy resin liquid, and uniformly sprinkles mixture powder on it, after suspension stands 4 hours, with not dipping in asphalt mixtures modified by epoxy resin
In one end insertion clay sand mold cavity bottom molding sand of rouge liquid, the depth being inserted into molding sand is 50mm, the top of pure aluminum metal silk
End maintains an equal level with type chamber top surface；
(4) it can be poured at this time with mould assembling, the pouring temperature of alloy is 680 DEG C, and the fine aluminium weight matched in master alloy liquid needs
The weight for getting rid of pure aluminum metal silk, 780 DEG C of heat preservation 20min after casting make mixture powder is evenly dispersed to enter in master alloy liquid,
After natural cooling, casting is taken out, casting is cut into the plate of thick 20mm；
(5) prewired aluminium alloy/ceramic powder is sent to plate upper surface as current-carrying gas using argon gas and is deposited
Region, current-carrying gas pressure are 0.2MPa, carrier flow 2.2L/min, powder feed rate 2g/min, and powder pushing precision reaches 0.1g/
Min then strikes off powder, layer thickness 5mm；
(6) deposition region, laser power 1.6KW, lasing beam diameter 20mm, scanning speed are strafed using optical fiber laser
5mm/s, positioning accuracy reach 0.1mm, and machining area fills argon gas and carries out inert gas shielding to 0.1MPa, and water oxygen content is down to
Lower than 100ppm, blowing argon gas is cooled to room temperature to form the first sedimentary after laser deposition processing；
(7) step (5) and (6) are repeated in the first deposition, forms the second sedimentary, continues to repeat in the second sedimentary
Step (5) and (6) form third sedimentary；
(8) by the plate solid solution aging containing three layers of gradient deposition layer: temperature is 480 DEG C of solid solution 60mim later in room temperature
It is cooling in water, then in 120 DEG C of timeliness 12h, it is again heated in 490 DEG C of temperature the 20h that homogenizes, is air-cooled to room temperature after taking-up；
(9) plate carries out making Nano surface, supersonic frequency 25kHz using ultrasonic surface rolling device after polishing polishing
Amplitude is 30 μm, load 300N when processing, and lathe revolving speed is 200r/min, feed speed 0.07mm/rev, ultrasonic surface
The hard alloy steel pellet impact 2.1 × 10 that every square millimeter of sample is 10mm by diameter after the completion of rolling4It is secondary；
(10) plate is put into chamber and is evacuated to 0.5 × 10-4, chamber is closed, chamber leak rate≤8Pa/h is measured；
It is passed through ammonia, the surface corrosion of third sedimentary is rinsed with 3w%NaOH and removes oxide skin(coating), after 45min, extracts the ammonia in furnace out,
And started to warm up after injecting high pure nitrogen to 500Pa, when sample surface temperature reaches 560 DEG C, nitriding 6h；
(11) cooled to room temperature takes out plate, heating plate to 300 DEG C of solid solution 1.5h, water cooling；It is heated to 100 DEG C
Timeliness 50h.
Gradient deposition layer, nitriding layer and aluminum alloy base material elemental analysis utilize 733 electron probe of JEOL SUPERPROBE
(El ectron Probe Microscopy-analyzer, EPMA) to composite material section carry out microcell (including line scanning or
Surface scan) analysis, study characteristic distributions of the element in composite material.Utilize PN5502 type X-ray energy spectrum (Energy
Distribution Sp ectroscopy EDS) and EDMAX energy spectrometer analysis alloy matrix aluminum and alumina-base material contained by element
Relative amount and characteristic distributions.
It measures and is evenly distributed with boron nitride, silica, tungstic acid, molybdenum disulfide mixture in the matrix in aluminium alloy
Particle, aluminium alloy matrix surface have three layers of continuous gradient deposition layer, and third deposition layer surface has nitriding layer；The gradient deposition
Layer with a thickness of 4mm, the nitrided case depth is 60 μm.
Embodiment 2: it is prepared as follows composite material:
One, the preparation of raw material:
Aluminium alloy/ceramic powder is by 80~95wt% alloy matrix aluminum powder and 5~20wt% ceramic powder
Composition, the ceramic material is by 25wt% silicon carbide, 25wt% diboron trioxide, 25wt% titanium boride, 20wt% silica,
5wt% calcium oxide composition；
The matrix composition of aluminium alloy is according to weight percentage are as follows: 0.5%Cu, 0.006%Au, 1.2%Mg, 0.07%
Pd, 0.08%Ni, 0.6%Zn, 0.4%Sr, 0.08%Ho, 8%Si, 0.07%Fe, 0.008%W, surplus Al.
Boron nitride in compound particles, silica, tungstic acid, molybdenum disulfide relative weight ratio be 1.4:1:1:
0.03, weight percent of the compound particles in alloy matrix aluminum is 5%, and the partial size of compound particles is 13 microns.
The aluminium alloy that first sedimentary uses/ceramic powder ingredient is 95wt% alloy matrix aluminum powder and 5wt%
Ceramic powder；The aluminium alloy that second sedimentary uses/ceramic powder ingredient for 88wt% alloy matrix aluminum powder and
12wt% ceramic powder；The aluminium alloy that third sedimentary uses/ceramic powder ingredient is 80wt% alloy matrix aluminum
Powder and 20wt% ceramic powder successively increase the ratio of ceramic material in the powder, so that combining between deposition of layers
Closely, using transient mode but also the combination between matrix and sedimentary more closely, is not easy stress removing.Aluminium alloy/pottery
The average grain diameter of ceramic material powder is 1mm.
Two, the preparation of composite material
(1) alloy matrix aluminum is put into melting in electrical crucible, smelting temperature is 830 DEG C, and heat preservation obtains after 70 minutes
Master alloy liquid, for use；Then weigh take boron nitride, silica, tungstic acid, molybdenum disulfide to be uniformly mixed to prepare mixture powder standby
With；
(2) clay sand mold is prepared by water, kaolin and zircon sand, and zircon sand partial size is 80 mesh, and kaolin is zircon sand
13wt%, kaolin and zircon sand are put into after sand mixer after dry-mixed 15min, are added zircon sand 11wt%'s in sand mixer
Water after continuing mixed grind 25 minutes, takes out moulding, shape forming cavity, sand mold bottom thickness 75mm.
(3) taking diameter is 6~8 millimeters of pure aluminum metal silk, and the length of silk is higher by 60 millimeters than type chamber height, by wire
Half length dip in epoxy resin liquid, and mixture powder is uniformly sprinkled on it, after suspension stands 6 hours, with not dipping in epoxy
In one end insertion clay sand mold cavity bottom molding sand of resin liquid, the depth being inserted into molding sand is 60mm, pure aluminum metal silk
Top and type chamber top surface maintain an equal level；
(4) it can be poured at this time with mould assembling, the pouring temperature of alloy is 710 DEG C, and the fine aluminium weight matched in master alloy liquid needs
The weight for getting rid of pure aluminum metal silk, 780 DEG C of heat preservation 40min after casting make mixture powder is evenly dispersed to enter in master alloy liquid,
After natural cooling, casting is taken out, casting is cut into the plate of thick 40mm；
(5) prewired aluminium alloy/ceramic powder is sent to plate upper surface as current-carrying gas using argon gas and is deposited
Region, current-carrying gas pressure are 0.2MPa, carrier flow 2.2L/min, powder feed rate 2g/min, and powder pushing precision reaches 0.1g/
Min then strikes off powder, layer thickness 7mm；
(6) deposition region, laser power 3.8KW, lasing beam diameter 40mm, scanning speed are strafed using optical fiber laser
9mm/s, positioning accuracy reach 0.1mm, and machining area fills argon gas and carries out inert gas shielding to 0.5MPa, and water oxygen content is down to
Lower than 100ppm, blowing argon gas is cooled to room temperature to form the first sedimentary after laser deposition processing；
(7) step (5) and (6) are repeated in the first deposition, forms the second sedimentary, continues to repeat in the second sedimentary
Step (5) and (6) form third sedimentary；
(8) by the plate solid solution aging containing three layers of gradient deposition layer: temperature is 500 DEG C of solid solution 60mim later in room temperature
It is cooling in water, then in 180 DEG C of 12~48h of timeliness, it is again heated in 490 DEG C of temperature the 30h that homogenizes, is air-cooled to after taking-up often
Temperature；
(9) plate carries out making Nano surface, supersonic frequency 40kHz using ultrasonic surface rolling device after polishing polishing
Amplitude is 30 μm, load 300N when processing, and lathe revolving speed is 200r/min, feed speed 0.07mm/rev, ultrasonic surface
The hard alloy steel pellet impact 3.5 × 10 that every square millimeter of sample is 10mm by diameter after the completion of rolling4It is secondary；
(10) plate is put into chamber and is evacuated to 1 × 10-4, chamber is closed, chamber leak rate≤8Pa/h is measured；It is logical
Enter ammonia, rinse third with 8w%NaOH and deposit layer surface, after 45min, extracts the ammonia in furnace out, and inject high pure nitrogen extremely
It is started to warm up after 700Pa, when sample surface temperature reaches 640 DEG C, nitriding 9h；
(11) cooled to room temperature takes out plate, heating plate to 400 DEG C of solid solution 1.5h, water cooling；It is heated to 110 DEG C
Timeliness 100h.
Gradient deposition layer, nitriding layer and aluminum alloy base material elemental analysis utilize 733 electron probe of JEOL SUPERPROBE
(El ectron Probe Microscopy-analyzer, EPMA) to composite material section carry out microcell (including line scanning or
Surface scan) analysis, study characteristic distributions of the element in composite material.Utilize PN5502 type X-ray energy spectrum (Energy
Distribution Sp ectroscopy EDS) and EDMAX energy spectrometer analysis alloy matrix aluminum and alumina-base material contained by element
Relative amount and characteristic distributions.
It measures and is evenly distributed with boron nitride, silica, tungstic acid, molybdenum disulfide mixture in the matrix in aluminium alloy
Particle, aluminium alloy matrix surface have three layers of continuous gradient deposition layer, and third deposition layer surface has nitriding layer；The gradient deposition
Layer with a thickness of 6mm, the nitrided case depth is 150 μm.
Embodiment 3: it is prepared as follows composite material:
One, the preparation of raw material:
Aluminium alloy/ceramic powder is by 80~95wt% alloy matrix aluminum powder and 5~20wt% ceramic powder
Composition, the ceramic material is by 33wt% silicon carbide, 20wt% diboron trioxide, 30wt% titanium boride, 15wt% silica,
2wt% calcium oxide composition；
The matrix composition of aluminium alloy is according to weight percentage are as follows: 0.3%Cu, 0.005%Au, 1.0%Mg, 0.055%
Pd, 0.065%Ni, 0.4%Zn, 0.3%Sr, 0.05%Ho, 5.5%Si, 0.055%Fe, 0.005%W, surplus Al.
Boron nitride in compound particles, silica, tungstic acid, molybdenum disulfide relative weight ratio be 1.25:1:1:
0.03, weight percent of the compound particles in alloy matrix aluminum is 4%, and the partial size of compound particles is 11.5 microns.
The aluminium alloy that first sedimentary uses/ceramic powder ingredient is 95wt% alloy matrix aluminum powder and 5wt%
Ceramic powder；The aluminium alloy that second sedimentary uses/ceramic powder ingredient for 88wt% alloy matrix aluminum powder and
12wt% ceramic powder；The aluminium alloy that third sedimentary uses/ceramic powder ingredient is 80wt% alloy matrix aluminum
Powder and 20wt% ceramic powder successively increase the ratio of ceramic material in the powder, so that combining between deposition of layers
Closely, using transient mode but also the combination between matrix and sedimentary more closely, is not easy stress removing.Aluminium alloy/pottery
The average grain diameter of ceramic material powder is 0.5mm.
Two, the preparation of composite material
(1) alloy matrix aluminum is put into melting in electrical crucible, smelting temperature is 820 DEG C, and heat preservation obtains after sixty minutes
Master alloy liquid, for use；Then weigh take boron nitride, silica, tungstic acid, molybdenum disulfide to be uniformly mixed to prepare mixture powder standby
With；
(2) clay sand mold is prepared by water, kaolin and zircon sand, and zircon sand partial size is 70 mesh, and kaolin is zircon sand
11wt%, kaolin and zircon sand are put into after sand mixer after dry-mixed 13min, are added zircon sand 10wt%'s in sand mixer
Water after continuing mixed grind 25 minutes, takes out moulding, shape forming cavity, sand mold bottom thickness 70mm.
(3) taking diameter is 7 millimeters of pure aluminum metal silk, and the length of silk is higher by 55 millimeters than type chamber height, by wire
Half length dips in epoxy resin liquid, and uniformly sprinkles mixture powder on it, after suspension stands 5 hours, with not dipping in asphalt mixtures modified by epoxy resin
In one end insertion clay sand mold cavity bottom molding sand of rouge liquid, the depth being inserted into molding sand is 55mm, the top of pure aluminum metal silk
End maintains an equal level with type chamber top surface；
(4) it can be poured at this time with mould assembling, the pouring temperature of alloy is 695 DEG C, and the fine aluminium weight matched in master alloy liquid needs
The weight for getting rid of pure aluminum metal silk, 780 DEG C of heat preservation 30min after casting make mixture powder is evenly dispersed to enter in master alloy liquid,
After natural cooling, casting is taken out, casting is cut into the plate of thick 30mm；
(5) prewired aluminium alloy/ceramic powder is sent to plate upper surface as current-carrying gas using argon gas and is deposited
Region, current-carrying gas pressure are 0.2MPa, carrier flow 2.2L/min, powder feed rate 2g/min, and powder pushing precision reaches 0.1g/
Min then strikes off powder, layer thickness 6mm；
(6) deposition region, laser power 2.7KW, lasing beam diameter 30mm, scanning speed are strafed using optical fiber laser
7mm/s, positioning accuracy reach 0.1mm, and machining area fills argon gas and carries out inert gas shielding to 0.3MPa, and water oxygen content is down to
Lower than 100ppm, blowing argon gas is cooled to room temperature to form the first sedimentary after laser deposition processing；
(7) step (5) and (6) are repeated in the first deposition, forms the second sedimentary, continues to repeat in the second sedimentary
Step (5) and (6) form third sedimentary；
(8) by the plate solid solution aging containing three layers of gradient deposition layer: temperature is 490 DEG C of solid solution 60mim later in room temperature
It is cooling in water, then in 150 DEG C of timeliness 30h, it is again heated in 490 DEG C of temperature the 25h that homogenizes, is air-cooled to room temperature after taking-up；
(9) plate carries out making Nano surface, supersonic frequency 33kHz using ultrasonic surface rolling device after polishing polishing
Amplitude is 30 μm, load 300N when processing, and lathe revolving speed is 200r/min, feed speed 0.07mm/rev, ultrasonic surface
The hard alloy steel pellet impact 2.8 × 10 that every square millimeter of sample is 10mm by diameter after the completion of rolling4It is secondary；
(10) plate is put into chamber and is evacuated to 0.7 × 10-4, chamber is closed, chamber leak rate≤8Pa/h is measured；
It is passed through ammonia, third is rinsed with 6w%NaOH and deposits layer surface, after 45min, extracts the ammonia in furnace out, and inject high pure nitrogen extremely
It is started to warm up after 600Pa, when sample surface temperature reaches 600 DEG C, nitriding 8h；
(11) cooled to room temperature takes out plate, heating plate to 350 DEG C of solid solution 1.5h, water cooling；It is heated to 105 DEG C
Timeliness 75h.
Gradient deposition layer, nitriding layer and aluminum alloy base material elemental analysis utilize 733 electron probe of JEOL SUPERPROBE
(El ectron Probe Microscopy-analyzer, EPMA) to composite material section carry out microcell (including line scanning or
Surface scan) analysis, study characteristic distributions of the element in composite material.Utilize PN5502 type X-ray energy spectrum (Energy
Distribution Sp ectroscopy EDS) and EDMAX energy spectrometer analysis alloy matrix aluminum and alumina-base material contained by element
Relative amount and characteristic distributions.
It measures and is evenly distributed with boron nitride, silica, tungstic acid, molybdenum disulfide mixture in the matrix in aluminium alloy
Particle, aluminium alloy matrix surface have three layers of continuous gradient deposition layer, and third deposition layer surface has nitriding layer；The gradient deposition
Layer with a thickness of 5mm, the nitrided case depth is 105 μm.
Comparative examples 1: remaining is same as Example 3, the difference is that carrying out the use used when laser deposition
Aluminium alloy/ceramic powder ingredient be 85wt% alloy matrix aluminum powder and 15wt% ceramic powder.And not into
The solid solution aging step of row step (8).
Comparative examples 2: a kind of wear-resisting aluminium is prepared according to the method that embodiment 1 in Chinese patent CN104109782A provides
Alloy, for the control in subsequent performance test.
It, will be in Examples 1 to 3 and comparative examples 1~2 in order to test the properties of wear-resistant material prepared by the present invention
The alloy material of preparation is tested as follows as sample:
(1) friction-wear test
At normal temperature, frictional wear experiment is carried out using ball disc type HT-1000 type abrasion tester.Gradient is shaped into block edge
Cut perpendicular to deposition direction, each gradient layer under three kinds of different conditions is cut into having a size of the resistance to of 28mm*15mm*8mm
Test specimen is ground, opposite grinding part is 15 steel ball (hardness 60HRC) of GCr, and diameter 6mm, sample is fixed on a spinstand, and opposite grinding steel ball exists
Specimen surface does the circular motion that radius is 6mm, normal load 5N, revolving speed 500r/min, and wearing- in period 20min is obtained and rubbed
Wipe coefficient curve.It before and after wear test, is required to carry out 10min ultrasonic cleaning to sample, with precision is 0.1mg after cleaning
Balance weigh to it, obtain wear weight loss.Its wear-resisting property of the smaller test specimen of wear weight loss is better, sample testing 3 times, takes
Average value.
1 abrasion resistance properties test result of table
The above results show that abrasion loss and coefficient of friction of the invention are substantially less than comparative examples 2, and embodiment 3 is each
Item data is considerably better than comparative examples 1, and layer-by-layer transition depositional mode is prompted to have certain contribution to wear-resisting property.And it compares
The properties of embodiment 1 are also considerably better than comparative examples 2, show that laser deposition ceramic material, which is added, to be also obviously improved
The wear-resisting property of basis material, but the effect of directly transition is good not as good as the wearability of layer-by-layer transition.
(2) functionally gradient material (FGM) bond strength is tested
Bond strength experiment is completed by cupping machine, the composite wood that will be prepared in embodiment 3 and comparative examples 1
Material first prepares the gradient deposition block having a size of 30*30*50mm, redeposited height on the basis of 20% ceramic layer of highest rate
For 100% alloy matrix aluminum of 16mm, deposition block is then cut into three pieces and does different heat treatment, processing post-tensioning examination respectively
Stick sampling, every kind of state take two test specimens, and test result is averaged.
The fracture position of test specimen is near 20% ceramic layer and alloy matrix aluminum binding site, this shows and gradient transition
Layer is compared, and the bond strength of direct transition zone is poor.Measure 3 test specimen average tensile strength 503Mpa of embodiment, elongation after fracture
About 2.2%, 1 tensile test specimen average tensile strength 312Mpa of comparative examples, elongation after fracture is about 2.7%, correlation data
It is found that the tensile strength of 3 test specimen of embodiment increases substantially, but plasticity reduces, after fixation rates, comparative examples
The tensile strength of 1 test specimen significantly reduces.Heat treatment can eliminate the residual stress of two kinds of materials, have to bond strength is improved
Very big help.
From experiment it can be seen that aluminium alloy/ceramic material can make to combine stronger a, side by the way of gradient transition
Face is performance mutation, and layer-by-layer transition alleviates two kinds of material heat expansions unevenness and the thermal stress of formation, and property gap is little, in conjunction with
More preferably.It on the other hand is porosity, the junction of oxide ceramics and aluminium alloy is easy to produce stomata, and with oxide ratio
The increase of example, the quantity and volume of stomata are also increased in tissue.
(3) neutral salt spray test
GB/T 10125-1997 (one salt spray test of artificial atmosphere corrosion test) is set using salt spray test according to national standards
The standby manual simulation's salt mist environment condition created determines product or metal salt fog resistance corrosive power.By sample by rule when experiment
Surely be exposed on the examination frame of the angle-style of salt spray test chamber, cover upper box lid subsequent start-up facility switching, from nozzle into cabinet by
The sodium chloride solution of upper and lower penetrating 5%, mist can equably be deposited in specimen surface, and controllable temperature is 35 ± 2 DEG C in case.
Sample is taken out after the test, is cleaned with deionized water, to remove the remaining salt fog solution of specimen surface, then uses hair dryer immediately
Drying judges corrosion proof quality by observing the situation of surface corrosion.The salt spray test time is set to 240 hours.
2 aluminium alloy neutral salt spray test of table
The addition of the above results surface, nitriding layer and gradient deposition layer can significantly resist the corrosiveness of salt fog, in protection
Layer basis material.
(4) micro-hardness testing
Forming block is cut along deposition direction, is tested on the side of test specimen using HVS-1000A type microhardness testers
Functionally gradient material (FGM) hardness number, loaded load 200g, load time 10s, test point are gradually transitioned into surface from matrix, and spacing is
1mm, each horizontal position are tested 3 times, and final result takes its average value.
| Group | Microhardness (HV0.2) |
| Embodiment 1 | 188 |
| Embodiment 2 | 174 |
| Embodiment 3 | 213 |
| Comparative examples 1 | 133 |
| Comparative examples 2 | 108 |
The above results show that the hardness of composite material prepared by the present invention is significantly higher than comparative examples 2, preferred embodiment
Hardness be up to 213HV0.2.Mainly due to the addition of the hybrid particles object of high rigidity, the deposition of the ceramic material on surface and
Ultrasonic surface rolling comprehensive function enhances the hardness of aluminum alloy base material.
In conclusion the hardness of boron nitride, silica, tungstic acid is high, the hardness and wearability of material are significantly improved, two
Antifriction quality can be improved in molybdenum sulfide.By adhering to boron nitride, silica, tungstic acid, molybdenum disulfide mixing on pure aluminum metal silk
The mode of composition granule so that mixed-powder is located at master alloy liquid center when casting, be conducive to the quick diffusion of micro powder granule with it is equal
Matter is homogenized without melt back, improves production efficiency.Zn, Sr, Ho improve the profit of aluminium alloy and foreign particles in alloy matrix aluminum
It is moist, it can be achieved that refined crystalline strengthening, i.e., the intensity of metal is improved by the refinement of crystallite size.Under external force, on crystal boundary
Dislocation pile up generate a stress field, can be used as the driving force started of dislocation source in activation neighboring die.Cu,Au,Mg,
Pd, Si, Al can realize solution strengthening, and alloying element, which is solid-solution in parent metal, causes a degree of distortion of lattice to make to close
The phenomenon that golden intensity improves.Ni, W, Fe can form dystectic compound, and Dispersed precipitate is in the base.Hardening constituent disperse is strong
The essence of change is that the movement of dislocation is hindered using the ultrafine dust of disperse, to improve the mechanical property of material.It is heavy by laser
Product aluminium alloy/ceramic powder forms three layers of gradient deposition layer, and effectively ceramic material and aluminum alloy materials are combined closely,
Sedimentary is fine and close and is tightly combined between layers, and the wearability of aluminum alloy base material can be obviously improved after composite deposition ceramic material
And corrosion resistance, the high temperature of laser deposition can also promote primary alumina particle in sedimentary, further promote hardness and wear-resisting
Property combines ceramic high-temperature resistant after composite material surface ceramic, and the low temperature resistant characteristic of metal applies the present invention
In needs while high temperature resistant and low temperature resistant part manufacture field.Surface carburization technique can further protect composite material table
Face enhances the corrosion resistance of composite material, and that improves material uses the time.Gradient deposition layer is carried out by nano surface technique
Ultrasonic surface rolling, the hardness and wearability on further reinforced composite material surface.
The above examples only illustrate the technical idea of the present invention, and this does not limit the scope of protection of the present invention, all
According to the technical idea provided by the invention, any changes made on the basis of the technical scheme each falls within the scope of the present invention
Within；The technology that the present invention is not directed to can be realized by the prior art.
Claims (7)
1. a kind of composite material, it is characterised in that: be evenly distributed with boron nitride, silica, three oxidations in the matrix of aluminium alloy
Tungsten, molybdenum disulfide compound particles, aluminium alloy matrix surface have three layers of continuous gradient deposition layer, and three layers of gradient deposition layer are by swashing
It is heavy to be followed successively by first according to deposition sequencing for light layer by layer deposition aluminium alloy/ceramic powder preparation on alloy matrix aluminum
Lamination, the second sedimentary, third sedimentary, aluminium alloy/ceramic powder by 80~95wt% alloy matrix aluminum powder and 5~
20wt% ceramic powder composition, the ceramic material is by 25~33wt% silicon carbide, 15~25wt% diboron trioxide, and 25
~35wt% titanium boride, 15~20wt% silica, 1~5wt% calcium oxide composition；The third deposition layer surface has nitriding
Layer；
The matrix composition of the aluminium alloy is according to weight percentage are as follows: 0.1-0.5%Cu, 0.004-0.006%Au, 0.8-
1.2%Mg, 0.04-0.07%Pd, 0.05-0.08%Ni, 0.2-0.6%Zn, 0.2-0.4%Sr, 0.02-0.08%Ho, 3-
8%Si, 0.04-0.07%Fe, 0.002-0.008%W, surplus Al.
2. a kind of composite material according to claim 1, it is characterised in that: boron nitride, oxygen in the compound particles
SiClx, tungstic acid, molybdenum disulfide relative weight ratio be 1.1-1.4:1:1:0.03, compound particles are in alloy matrix aluminum
Weight percent be 3-5%, the partial sizes of compound particles is 10-13 microns.
3. a kind of composite material according to claim 1, it is characterised in that: the aluminium that first sedimentary uses closes
Gold/ceramic powder ingredient is 95wt% alloy matrix aluminum powder and 5wt% ceramic powder；Second sedimentary is adopted
Aluminium alloy/ceramic powder ingredient is 88wt% alloy matrix aluminum powder and 12wt% ceramic powder；Described
The aluminium alloy that three sedimentaries use/ceramic powder ingredient is 80wt% alloy matrix aluminum powder and 20wt% ceramic material powder
End.
4. a kind of composite material according to claim 3, it is characterised in that: the aluminium alloy/ceramic powder
Average grain diameter is 0.1~1mm, the gradient deposition layer with a thickness of 4~6mm, the alloy matrix aluminum with a thickness of 20~
40mm, the nitrided case depth are 60~150 μm.
5. a kind of preparation method of the composite material as described in any one of Claims 1 to 4, which is characterized in that include following tool
Body step:
(1) alloy matrix aluminum is put into melting in electrical crucible, smelting temperature is 810~830 DEG C, after heat preservation 50-70 minutes
Master alloy liquid is obtained, for use；Then it weighs and takes boron nitride, silica, tungstic acid, molybdenum disulfide are uniformly mixed to prepare mixture
Powder is spare；
(2) taking diameter is 6~8 millimeters of pure aluminum metal silk, and the length of silk is higher by 50~60 millimeters than type chamber height, by wire
Half length dip in epoxy resin liquid, and mixture powder is uniformly sprinkled on it, after suspension stands 4~6 hours, with not dipping in ring
In one end insertion clay sand mold cavity bottom molding sand of oxygen resin liquid, the depth being inserted into molding sand is 50~60mm, fine aluminium gold
The top and type chamber top surface for belonging to silk maintain an equal level；
(3) it can be poured at this time with mould assembling, the pouring temperature of alloy is 680~710 DEG C, and the fine aluminium weight matched in master alloy liquid needs
The weight for getting rid of pure aluminum metal silk, 780 DEG C of 20~40min of heat preservation after casting make mixture powder is evenly dispersed to enter female close
In golden liquid, after natural cooling, casting is taken out, casting is cut into the plate of 20~40mm of thickness；
(4) prewired aluminium alloy/ceramic powder is sent to plate upper surface deposition region as current-carrying gas using argon gas,
Powder pushing precision reaches 0.1g/min, then strikes off powder, and layer thickness is 5~7mm；
(5) deposition region, 1.6~3.8KW of laser power are strafed using optical fiber laser, lasing beam diameter is 20~40mm, is swept
5~9mm/s of speed is retouched, positioning accuracy reaches 0.1mm, and machining area fills argon gas to 0.1~0.5MPa progress inert gas guarantor
Shield, water oxygen content are brought down below 100ppm, and blowing argon gas is cooled to room temperature to form the first sedimentary after laser deposition processing；
(6) step (4) and (5) are repeated in the first sedimentary, form the second sedimentary, continue to repeat to walk in the second sedimentary
Suddenly (4) and (5) form third sedimentary；
(7) by the plate solid solution aging containing three layers of gradient deposition layer: temperature is 480~500 DEG C of solid solution 60mim later in room temperature
It is cooling in water, then in 120~180 DEG C of 12~48h of timeliness, the 20~30h that homogenizes is again heated in 490 DEG C of temperature, after taking-up
It is air-cooled to room temperature；
(8) plate carries out making Nano surface, 25~40kHz of supersonic frequency using ultrasonic surface rolling device after polishing polishing
Amplitude is 30 μm, load 300N when processing, and lathe revolving speed is 200r/min, feed speed 0.07mm/rev, ultrasonic surface
The hard alloy steel pellet impact 2.1~3.5 × 10 that every square millimeter of sample is 10mm by diameter after the completion of rolling4It is secondary；
(9) plate is put into chamber and is evacuated to 0.5~1 × 10-4, chamber is closed, chamber leak rate≤8Pa/h is measured；It is logical
Enter ammonia, rinse third with 3~8w%NaOH and deposit layer surface, after 45min, extracts the ammonia in furnace out, and inject high pure nitrogen
It is started to warm up after to 500~700Pa, when sample surface temperature reaches 560~640 DEG C, 6~9h of nitriding；
(10) cooled to room temperature takes out plate, heating plate to 300~400 DEG C of solid solution 1.5h, water cooling；It is heated to 100~
110 DEG C of 50~100h of timeliness.
6. a kind of preparation method of composite material according to claim 3, it is characterised in that: the clay sand mold by
Water, kaolin and zircon sand preparation, zircon sand partial size are 60-80 mesh, and kaolin is the 9-13wt% of zircon sand, by kaolin and
Zircon sand is put into after sand mixer after dry-mixed 10-15min, and the water of zircon sand 9-11wt% is added in sand mixer, continues mixed grind 20-
After 25 minutes, moulding, shape forming cavity, sand mold bottom 65~75mm of thickness are taken out.
7. a kind of preparation method of composite material according to claim 3, it is characterised in that: the current-carrying gas pressure
For 0.2MPa, carrier flow 2.2L/min, powder feed rate 2g/min.
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