CN101748348B - Method for preparing high-performance ceramic particle reinforced metal base composites - Google Patents

Method for preparing high-performance ceramic particle reinforced metal base composites Download PDF

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Publication number
CN101748348B
CN101748348B CN2009103109448A CN200910310944A CN101748348B CN 101748348 B CN101748348 B CN 101748348B CN 2009103109448 A CN2009103109448 A CN 2009103109448A CN 200910310944 A CN200910310944 A CN 200910310944A CN 101748348 B CN101748348 B CN 101748348B
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ceramic particle
crucible
preparing
vacuum
particle
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CN101748348A (en
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高文理
苏海
张辉
曾佩兰
陈江华
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SHANDONG RUIYE FLANGE CO., LTD.
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Hunan University
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Abstract

The invention relates to a method for preparing high-performance ceramic particle reinforced metal base composites, comprising the following steps: 1. taking ceramic particles, removing impurities on particle surfaces and then chemically plating metallic copper or nickel on the surfaces; 2. gradually adding the ceramic particles in an alloy liquid surface, and at the same time using a stirrer for level-wise speeding-up stirring to a fused mass; 3. putting a vacuum cover on a crucible for vacuum degassing to the composite fused mass in the crucible; while in the vacuum degassing, low-speed stirring the composite fused mass in the crucible, discharging, and pouring preparing metal base composite ingot blanks. In the method, the inner surface of the crucible is provided with a graphite layer. The invention has the advantages of simple process, easy operation, short process flow, stable process, good combination of particles and alloy matrix interfaces, good stirring effect, uniform distribution of particles in alloy matrix, low porosity of composites, high performance and low cost of production, and is suitable for preparing high-performance ceramic particle reinforced metal base composites in an industrial scale.

Description

A kind of method for preparing high-performance ceramic particle reinforced metal base composites
Technical field
The present invention relates to the preparation method of particles reiforced metal-base composition, be meant a kind of method for preparing high-performance ceramic particle reinforced metal base composites especially, belong to metallurgical technology field.
Background technology
Ceramic particle reinforced aluminium base composite material has high specific tenacity, high specific modulus, and thermal expansivity is little, and advantages such as good temperature resistance and wear resistance, has been widely used in fields such as aerospace, communications and transportation as the lightweight structure material at present.In recent years, along with the fast development of domestic air mail space flight and automobile, electron trade, the demand of particle enhanced aluminum-based composite material is increased just year by year.At present, the preparation technology of particle enhanced aluminum-based composite material has methods such as powder metallurgy, extrusion casting, spray co deposition and stirring casting.Stirring casting method has that production cost is low, and equipment is simple, and technical process is short, and characteristics such as productivity height are comparatively ideal methods of high-performance ceramic particle reinforced metal base composites industrial-scale production.
The mechanical stirring casting is meant earlier matrix alloy to be placed in the crucible and melts; Under liquid state or semi-solid state, stir; And add while stirring or disposable adding pottery enhancing body particle, uniform particles is distributed in the matrix metal, thereby prepares composite material sizing agent.Then, the needs according to using carry out extrusion casting, low-pressure casting, adjustable pressure casting with composite material sizing agent, or the matrix material ingot casting are carried out follow-up hot extrusion and rolling deformation, thereby obtain composite product.There is following problem in stirring casting method: 1. ceramic particle and alloy melt wettability are relatively poor, and the two is difficult to compound; 2. the alloy melt surface tension is big, and particle is difficult to be uniformly distributed in the matrix alloy after getting into melt; 3. in the whipping process, be involved in gas in the melt easily, and cause void content higher; 4. serious surface reaction takes place in ceramic particle and alloy melt easily.At present, disclosed stirring casting method prepares the technology of preparing of metal-base composites for addressing the above problem, and major measure has: through improving stirring velocity; Make the powerful entering of particle alloy melt, and stirring velocity is too high, particle flies upward excessive at the alloy liquid level; Cause particulate content inaccurate; And, melt volume gas, slag inclusion is also more serious; Adopt complete vacuum apparatus that whipping process is carried out vacuum protection, but this will require equipment to have higher elevated-temperature seal property, and simultaneously, cause production cost to improve.In addition; Because it is more abominable to stir the whole working condition of recombination process, the melt flow field in the crucible can not understood in depth, in crucible and agitator structure design; Usually there is not substantial theoretical direction; Cause at last existing in the crucible and stir " dead band " or " stagnant wake ", strengthen the body particle and reunite in these zones easily, stir composite effect and descend.At present, the common cast-iron pot of the most of use of disclosed crucible under the washing away of hot conditions and melt, causes impurity level increases such as matrix material iron content, worsens the mechanical property of material.And disclosed appliance arrangement operation is to be accomplished by manual work basically, and production process relies on manual work to control by rule of thumb, and accidentalia is more, causes material structure inhomogeneous, unstable properties, and process repeatability is poor.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art and provide that a kind of process method is simple, easy to operate, technical process weak point, process stabilizing, particle and alloy substrate interface junction get togather, stir that composite effect is good, particle uniform distribution, matrix material void content in alloy substrate is low, excellent performance, the method for preparing high-performance ceramic particle reinforced metal base composites that production cost is low.
The present invention---a kind of method for preparing high-performance ceramic particle reinforced metal base composites comprises the steps:
The first step: ceramic grain surface pre-treatment
Get ceramic particle, surface chemical metal plating behind the removal particle surface impurity;
Second step: ceramic particle mixes with alloy melt
Be incubated after the metallic matrix alloy placed crucible heat fused, refining; The first step is handled the ceramic particle that obtains progressively add the alloy liquid level, simultaneously, carrying out step by step with whisking appliance to melt, raising speed stirs; Initial stirring velocity is: 250~300 rev/mins; When stirring velocity progressively is increased to 550~650 rev/mins with 15~30 rev/mins speed, continue to stir 2~8 minutes, stop to add ceramic particle; Then, stirring velocity is risen to 1200~1500 rev/mins, melt is carried out brute force stirred 3~8 minutes, last, stirring velocity is reduced to 450~550 rev/mins, stirred 2~8 minutes, stop to stir;
The 3rd step: vacuum stripping
The mixed melt temperature places vacuum (-tight) housing on the crucible at 700-720 ℃ in the control crucible, is evacuated to 0.01-0.04Mpa; Compounding flux in the crucible is carried out vacuum stripping; Vacuum stripping time: 5-15min in the vacuum degassed while, makes whisking appliance carry out stirring at low speed with the stirring velocity of 100-200r/min to the compounding flux in the crucible; Come out of the stove cast preparation metal-base composites ingot blank.
Among the present invention, describedly be meant in ceramic grain surface copper facing or nickel plating at the ceramic grain surface chemical plating metal.
Among the present invention, described ceramic grain surface copper-plating technique condition is:
Solution composition is: add in the per kilogram water: copper sulfate 15-20g; Seignette salt 40-50g; Sodium hydroxide 10-15g; Formaldehyde 13-20ml forms; Ceramic particle is placed in the plating bath through decontamination one alligatoring one sensitization one activation, and plating time is: 10~18min; Then, after the ceramic particle vacuum-drying with copper coating, be the composite granule of copper coated silicon carbide pottery.
Among the present invention, described ceramic grain surface nickel plating technology condition is:
Solution composition is: single nickel salt 30g/L, inferior sodium phosphate 20g/L, hydrofluoric acid (40%) 10mL/L, matt salt 10g/L, NH 3H 2O30mL/L; The pH value of coordination agent control plating bath is about 6.5; Bath temperature: 80 ± 5 ℃; Ceramic particle is placed in the plating bath through alkaline degreasing one acid etching one sensitization one activation, and plating time is: 10~18min; Then, after the ceramic particle vacuum-drying behind the plating nickel on surface, be the composite granule that nickel coats silicon carbide ceramics.
Among the present invention, said inner surface of crucible is lined with graphite linings, and said graphite linings thickness is 5~10 millimeters.
Among the present invention; Said whisking appliance is multistage blade agitators; Said blade progression: (rounding); In the formula: n--blade progression, H--melt height.
Among the present invention, the blade of said whisking appliance is the plane, and said blade diameter is 0.5-0.7 with the crucible diameter ratio; Said blade normal and stir shaft axis angle are α, 30 °≤α≤60 °.
The present invention has following useful effect owing to adopt above-mentioned process method
1, ceramic particle has improved the wettability of particle and alloy melt effectively through the surface metalation pre-treatment, and it is compound to help the two stirring.
2, classification is stirred, and helps ceramic particle and gets into fast in the matrix metal melt, and high speed subsequently is powerful to be stirred; The efficient radial effect power that produces; The thorough mixing that helps particle and melt, and can break up particle powder group effectively, further improve particle dispersed uniform property in melt; Subsequently, compounding flux is carried out vacuum stripping; Under the cooperation of low-speed agitator, break the sull of compounding flux liquid level, bubble is overflowed in melt easily, thereby reduced the void content of matrix material, and improve the combination of Al/SiC interface effectively, improve performance of composites.
3, the used crucible of the present invention adopts liner graphite linings technology, has avoided melt and irony Long contact time, has washed away, and effectively reduces in the compounding flux foreign matter contents such as iron, increases substantially the mechanical property of material.
4, confirm whisking appliance progression according to shape, size and the alloy melt height of stirring crucible; Confirm the angle of blade diameter and blade and stir shaft according to crucible diameter; Effectively improved the stirring and mixing effect of whisking appliance; Effectively eliminate and stir dead band and stagnant wake, make particle uniform distribution in alloy substrate.
In sum; Process method of the present invention is simple, easy to operate, technical process weak point, process stabilizing, particle and the alloy substrate interface junction gets togather, mixing effect is good, particle uniform distribution, matrix material void content in alloy substrate is low, excellent performance, production cost are low, is suitable for industrially scalable and prepares high-performance ceramic particle reinforced metal base composites.
Description of drawings
Accompanying drawing 1 is the structural representation of whisking appliance among the present invention.
Accompanying drawing 2 is SiC particle distribution and interface scanning electromicroscopic photograph in the body alloy of the embodiment of the invention 1 products therefrom.
Accompanying drawing 3 is SiC particle distribution and interface scanning electromicroscopic photograph in the body alloy of the embodiment of the invention 2 products therefroms.
Accompanying drawing 4 is SiC particle distribution and interface scanning electromicroscopic photograph in the body alloy of the embodiment of the invention 3 products therefroms.
In the accompanying drawing 1: 1---buncher, 2---stir shaft, 3---agitating vane.
The stereoscan photograph of accompanying drawing 2,3,4 can find out that obviously the SiC particle is evenly distributed in metallic matrix, SiC/Al interface bond quality is good.
Embodiment
Strengthen the body particle with the SiC particle as pottery, the A356 duraluminum is a matrix alloy, at first, gets granularity and is: the SiC particle of 10um-15um, at ceramic grain surface chemical plating metal copper, nickel; Concrete technology is following:
A, ceramic grain surface copper-plating technique condition are:
Solution composition is: add in the per kilogram water: copper sulfate 15-20g; Seignette salt 40-50g; Sodium hydroxide 10-15g; Formaldehyde 13-20ml forms; Ceramic particle is placed in the plating bath plating time through decontamination one alligatoring one sensitization one activation: 10~18min; Then, after the ceramic particle vacuum-drying with copper coating, be the composite granule of copper coated silicon carbide pottery.
B, ceramic grain surface nickel plating technology condition are:
Solution composition is: single nickel salt 30g/L, inferior sodium phosphate 20g/L, hydrofluoric acid (40%) 10mL/L, matt salt 10g/L, NH 3H 2O30mL/L; The pH value of coordination agent control plating bath is about 6.5; Bath temperature: 80 ± 5 ℃; Ceramic particle is placed in the plating bath plating time through alkaline degreasing one acid etching one sensitization one activation: 10~18min; Then, after the ceramic particle vacuum-drying with plating nickel on surface, be the composite granule that nickel coats silicon carbide ceramics.
Following three specific embodiments are provided then.
Embodiment 1
Get aluminium ingot 8.5Kg and place crucible, smelting temperature is controlled at 690~700 ℃, treats to melt fully, adds alloying element respectively; As: silicon, copper, magnesium etc.; Skim after the alloying element fusing, then alloy melt is carried out the argon gas refining, control alloy melt temperature is: 620-650 ℃; In the duraluminum alloy melt, feed argon gas, argon flow amount is: 1-2.5L/min, degasification time: 10-20min.Keeping the aluminium alloy melt temperature is 620-650 ℃, in crucible, feeds rare gas element, and under protection of inert gas, the composite granule 1.5Kg that copper coated silicon carbide is ceramic progressively joins melt liquid level through feed hopper; Start buncher, make the initial stirring velocity of whisking appliance be: 250 rev/mins, when stirring velocity progressively is increased to 550 rev/mins with 15 rev/mins speed, continue to stir 2 minutes, stop to add ceramic particle; Then, stirring velocity is risen to 1200 rev/mins, melt is carried out brute force stirred 3 minutes, radial effect power helps the thorough mixing of particle and melt efficiently, and can break up particle powder group effectively, realizes particle homodisperse in melt.Powerful stir finish after, stirring velocity is reduced to 450 rev/mins, stirred 2 minutes, stop to stir, with steady melt flow field gradually.The whole charging process roughly needs 20min.Then, vacuum (-tight) housing is placed on the crucible, compounding flux is carried out vacuum stripping handle; The degassing process parameter is: the compounding flux temperature is risen to: 700 ℃; Vacuum tightness: 0.01-0.04Mpa, and start whisking appliance, stirring velocity is 100r/min, the vacuum stripping time: 5min.Shed vacuum (-tight) housing, come out of the stove, casting.Through detecting, the SiC particle is distributed in the metallic matrix more equably, and there is reunion in the subregion and gathers phenomenon partially, and impurity such as pore and iron are less, and SiC/Al interface bond quality is good, and the as cast condition Tensile strength is 145-155MPa.
Embodiment 2
Get aluminium ingot 8.5Kg and place crucible, smelting temperature is controlled at 690~700 ℃, treats to melt fully, adds alloying element respectively; As: silicon, copper, magnesium etc.; Skim after the alloying element fusing, then alloy melt is carried out the argon gas refining, control alloy melt temperature is: 620-650 ℃; In the duraluminum alloy melt, feed argon gas, argon flow amount is: 1-2.5L/min, degasification time: 10-20min.Keeping the aluminium alloy melt temperature is 620-650 ℃, in crucible, feeds rare gas element, under protection of inert gas, will progressively join melt liquid level through feed hopper through the SiC of Electroless copper ceramic particle 1.5Kg; Start buncher, make the initial stirring velocity of whisking appliance be: 270 rev/mins, when stirring velocity progressively is increased to 600 rev/mins with 23 rev/mins speed, continue to stir 5 minutes, stop to add ceramic particle; Then, stirring velocity is risen to 1350 rev/mins, melt is carried out brute force stirred 5 minutes, radial effect power helps the thorough mixing of particle and melt efficiently, and can break up particle powder group effectively, realizes particle homodisperse in melt.Powerful stir finish after, stirring velocity is reduced to 500 rev/mins, stirred 5 minutes, stop to stir, with steady melt flow field gradually; The whole charging process roughly needs 15min.Vacuum (-tight) housing is placed on the crucible, compounding flux is carried out vacuum stripping handle; The degassing process parameter is: the compounding flux temperature is risen to: 710 ℃; Vacuum tightness: 0.01-0.04Mpa, and start whisking appliance, stirring velocity is 150r/min, the vacuum stripping time: 10min.Shed vacuum (-tight) housing, come out of the stove, casting.Through detecting, the SiC uniform particles is distributed in the metallic matrix, does not have obviously reunion and gathers phenomenon partially, and impurity such as pore and iron are less, and the interface bond quality is good, and the as cast condition Tensile strength can reach 180MPa.
Embodiment 3
Get aluminium ingot 8.5Kg and place crucible, smelting temperature is controlled at 690~700 ℃, treats to melt fully, adds alloying element respectively; As: silicon, copper, magnesium etc.; Skim after the alloying element fusing, then alloy melt is carried out the argon gas refining, control alloy melt temperature is: 620-650 ℃; In the duraluminum alloy melt, feed argon gas, argon flow amount is: 1-2.5L/min, degasification time: 10-20min.Keeping the aluminium alloy melt temperature is 620-650 ℃, in crucible, feeds rare gas element, under the protection of rare gas element, will progressively join melt liquid level through feed hopper through the SiC of chemical nickel plating on surface ceramic particle 1.5Kg; Start buncher, make the initial stirring velocity of whisking appliance be: 300 rev/mins, when stirring velocity progressively is increased to 600 rev/mins with 30 rev/mins speed, continue to stir 8 minutes, stop to add ceramic particle; Then, stirring velocity is risen to 1500 rev/mins, melt is carried out brute force stirred 8 minutes, radial effect power helps the thorough mixing of particle and melt efficiently, and can break up particle powder group effectively, realizes particle homodisperse in melt.Powerful stir finish after, stirring velocity was reduced to 550/ minute, stirred 8 minutes, stop to stir, with steady melt flow field gradually; The whole charging process roughly needs 10min; Vacuum (-tight) housing is placed on the crucible, compounding flux is carried out vacuum stripping handle; The degassing process parameter is: the compounding flux temperature is risen to: 720 ℃; Vacuum tightness: 0.01-0.04Mpa, and start whisking appliance, stirring velocity is 200r/min, the vacuum stripping time: 15min.Shed vacuum (-tight) housing, come out of the stove, casting.Through detecting, the SiC uniform particles is distributed in the metallic matrix, does not have obviously reunion and gathers phenomenon partially, and impurity such as pore and iron are less, and SiC/Al interface bond quality is good, and the as cast condition Tensile strength is 170-180MPa.

Claims (4)

1. a method for preparing SiC ceramic particle reinforced Al matrix composite comprises the steps:
The first step: ceramic grain surface pre-treatment
Get the SiC ceramic particle, Electroless copper or nickel plating metal behind the removal particle surface impurity;
Second step: ceramic particle mixes with alloy melt
Be incubated after the metallic matrix duraluminum placed crucible heat fused, refining; The first step is handled the ceramic particle that obtains progressively add the alloy liquid level, simultaneously, carrying out step by step with whisking appliance to melt, raising speed stirs; Initial stirring velocity is: 250~300 rev/mins; When stirring velocity progressively is increased to 550~650 rev/mins with 15~30 rev/mins speed, continue to stir 2~8 minutes, stop to add ceramic particle; Then, stirring velocity is risen to 1200~1500 rev/mins, melt is carried out brute force stirred 3~8 minutes, last, stirring velocity is reduced to 450~550 rev/mins, stirred 2~8 minutes, stop to stir, obtain the compounding flux of SiC and duraluminum; Said whisking appliance is multistage blade agitators; Said blade progression: in formula: n--blade progression rounds; The H---melt height; The blade of said whisking appliance is the plane, and said blade diameter is 0.5-0.7 with the crucible diameter ratio; Said blade normal and stir shaft axis angle are α, 30 °≤α≤60 °.
The 3rd step: vacuum stripping
The compounding flux temperature places vacuum (-tight) housing on the crucible at 700-720 ℃ in the control crucible, is evacuated to 0.01-0.04MPa; Compounding flux in the crucible is carried out vacuum stripping; Vacuum stripping time: 5-15min in the vacuum degassed while, makes whisking appliance carry out stirring at low speed with the stirring velocity of 100-200r/min to the compounding flux in the crucible; Come out of the stove cast preparation metal-base composites ingot blank.
2. a kind of method for preparing high-performance ceramic particle reinforced metal base composites according to claim 1 is characterized in that: described technology at ceramic grain surface chemical plating metal copper is:
Solution composition is: add in the per kilogram water: copper sulfate 15-20g; Seignette salt 40-50g; Sodium hydroxide 10-15g; Formaldehyde 13-20ml forms; Ceramic particle is placed in the plating bath through decontamination one alligatoring one sensitization one activation, and plating time is: 10~18min; Then, after the ceramic particle vacuum-drying with copper coating, be the copper coated silicon carbide ceramic particle.
3. a kind of method for preparing high-performance ceramic particle reinforced metal base composites according to claim 1 is characterized in that: described technology at ceramic grain surface chemical plating metal nickel is:
Solution composition is: single nickel salt 30g/L, and inferior sodium phosphate 20g/L, concentration is 40% hydrofluoric acid 10mL/L, matt salt 10g/L, NH 3H 2O30mL/L; The pH value of coordination agent control plating bath is about 6.5; Bath temperature: 80 ± 5 ℃; Ceramic particle is placed in the plating bath through alkaline degreasing one acid etching one sensitization one activation, and plating time is: 10~18min; Then, after the ceramic particle vacuum-drying behind the plating nickel on surface, be nickel and coat the silit ceramic particle.
4. a kind of method for preparing high-performance ceramic particle reinforced metal base composites according to claim 1, it is characterized in that: said inner surface of crucible is lined with graphite linings, and said graphite linings thickness is 5~10 millimeters.
CN2009103109448A 2009-12-04 2009-12-04 Method for preparing high-performance ceramic particle reinforced metal base composites Active CN101748348B (en)

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