CN109112335A - A kind of nano aluminum nitride enhances the hot-press method of 7075 aluminium alloys - Google Patents
A kind of nano aluminum nitride enhances the hot-press method of 7075 aluminium alloys Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0068—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only nitrides
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
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Abstract
A kind of nano aluminum nitride enhances the hot-press method of 7075 aluminium alloys, under acidic environment, using sensitizing solution in nano-aluminum nitridenpAdsorption Sn2+Ion, and obtain in later period activation process with nano-aluminum nitridenpFor core, the Pd-Sn of adsorption is the core-shell particles at electroless plating reaction center, finally obtains Cu cladding nano-aluminum nitride by chemical platingnpParticle.Gained powder and 7075 Al alloy powders are obtained being cold-pressed blank in required ratio mixing and ball milling and cold pressing.Cold pressing blank is put into graphite jig and carries out vacuum heating-press sintering.Gained hot pressing blank is subjected to plasticity thermal deformation field by heat extruder, extrusion billet is obtained, then extrusion billet is subjected to Equal Channel Angular Pressing processing again, obtains premium quality product.Product prepared by the present invention has excellent mechanical performance, meanwhile, the present invention has many advantages, such as simple, safe, easily operated and controllable.
Description
Technical field
The invention belongs to technical field of material.
Background technique
Particle enhanced aluminum-based composite material has that light-weight, specific strength is high, the high and low density of specific stiffness, wearability and low
The advantages that cost and become one of very promising new material, thus in auto industry, aerospace, electronics, military project, sport
It is widely used etc. many fields.Wherein, aluminium nitride reinforced aluminum matrix composites become standby in metal-base composites
It attracts attention, the composite material that most study, potential application are most wide.
Largely the study found that the mechanical property of composite material is with enhancing when the size of reinforcement reaches micron order
The increase of body content and decline, weaker combination interface and because reinforcement reunite due to induce crackle roughening cause performance decline
Main cause.In recent years, there is researcher's discovery, the reinforcement that a small amount of nano-scale is added can greatly improve composite material
Mechanical property, such as: higher specific strength, preferable high-temperature behavior, creep resistant, anticorrosive etc..
With making rapid progress for metal-base composites preparation means, the various problems in preparation process also expose nothing
Lose, for example, on interface brittlement phase precipitation, strong interfacial reaction leads to the loss of reinforcement, and the pattern of reinforcement is to composite wood
Expect the influence of comprehensive performance, the load transmission etc. between reinforcement and matrix.The interface of composite material is almost in these problems
It is an eternal topic.Meanwhile in the composite material preparation process of liquid phase participation, the wetability of liquid-solid two-phase seems outstanding
To be important, on the one hand determine the complexity of composite material preparation, on the other hand reflect the comprehensive of composite material indirectly again
Close performance.For nano particle, biggish body surface is poor than the Van der Waals force between, nano particle and with metal bath
Wetability make a nanometer reinforcement be difficult to be evenly distributed and be dispersed in metal bath.Therefore, the entire composite material of overall view
Preparation process, the research for interface problem and wetability is the premise and basis of the excellent composite material of processability.
In publication 106350753B, title are as follows: a kind of " simple substance copper clad whisker carbon nanotube/magnesium-based composite wood
Expect the preparation method of semi-solid blank " in.Carbon nanotube is pre-processed using chemisorption to obtain copper-plated carbon nanotube.
It is re-introduced into ultrasonic disperse and founding obtains composite material.In fact this method due to chemisorption limitation, to human injury
It is larger, and it also requires the production cycle is long individually to carbon nanotube carboxylated, it is at high cost, it is unfavorable for large batch of production, has
Certain limitation.
In publication 104532032A, title are as follows: " one kind prepares nano aluminium oxide enhancing based on complex vibration technology
In the method for aluminum matrix composite semi solid slurry ".Nano aluminium oxide is located in advance using the mechanical alloying effect of ball milling
Reason obtains the composite particles of cladding Mg.It is re-introduced into ultrasonic disperse and founding obtains composite material.In fact this method due to Mg with
Nano aluminium oxide is combined by physical mechanical mode, and bond strength is weaker, and covered effect is simultaneously bad, is brought for subsequent production
Certain randomness.
Summary of the invention
The purpose of the present invention is to propose to the hot-press methods that a kind of nano aluminum nitride enhances 7075 aluminium alloys.
The present invention coats one layer of metallic copper in nano silicon nitride aluminium surface using electroless plating method, in ball milling and the mistake of vacuum hotpressing
In journey nanometer reinforcing phase is evenly dispersed in matrix, and is had excellent performance by thermoplastic extrusion and Equal Channel Angular Pressing
Product.This method is at low cost, can produce in enormous quantities.Meanwhile being formed by Al/AlNnpInterface is stablized by metal copper layer ties
It closes, binding performance is preferable, and resulting composite material crystal grain is tiny, and mechanical performance is excellent.
Cu coats nano-aluminum nitride during hot pressingnpThe content of particle, the control of environment and the determination of technological parameter are non-
Often important, these three links are all linked with one another, all directly affect the quality of product.
Concrete principle of the invention are as follows: by the mechanical stirring of high-energy ball milling and the plastic flow of vacuum hotpressing, by Cu packet
Cover nano-aluminum nitridenpParticle uniformly diffuses to melt.Nano-aluminum nitride is coated to reduce nanometer CunpThe reunion situation of particle, passes through chemistry
Plating method is to nano-aluminum nitridenpSurface is handled, its surface is made to be coated with amorphous metal copper as stable particle protective layer.Together
When, it, can effectively REINFORCED Al/AlN during vacuum hotpressingnpInterface bond strength makes nano-aluminum nitridenpMore stable fixation
In the base.In addition, in extrusion process using shearing force crush crystal grain, and cause dislocation to tangle for composite material dynamic again
Crystallization provides driving force, achievees the purpose that refine crystal grain.It can effectively disperse to increase during carrying out Equal Channel Angular Pressing processing
Strong phase and interphase, to obtain the product of excellent mechanical properties.
The present invention is achieved by the following technical solutions.
A kind of nano aluminum nitride of the present invention enhances the hot-press method of 7075 aluminium alloys, includes the following steps.
(1) by nano-aluminum nitridenpIt is placed in 10%NaOH solution to boil and keeps 30min, filter off NaOH solution, use deionized water
Particle is constantly rinsed until pH value be in neutrality, filtering drying.
(2) particle in step (1) is put into concentrated hydrochloric acid and is boiled 30 minutes, carried out roughening treatment, then use deionization
Water cleaning, drying.
(3) step (2) obtained particle is placed in mechanical stirring 10min in sensitizing solution, wherein sensitizing solution proportion is
SnCl2•2H2O:HCl:NaCl:H2O=10g:20ml:25g:100g。
(4) activating solution is added in the particle in step (3), stirs 10min, stands later, wherein the proportion of activating solution is
PdCl2: hydrochloric acid: H2O=1g:50ml:100g.After powder precipitating, filtering, then powder is washed with deionized.
(5) in the ratio of 10g:90~100ml, by CuSO4•5H2O is dissolved in distilled water, stirring and dissolving, is obtained clear
Blue solution A；In the ratio of 60g:100ml, sodium potassium tartrate tetrahydrate is dissolved in distilled water, stirring and dissolving, obtains colourless clarification
Solution B.In the case of stirring, the B liquid of equivalent is poured into A liquid and obtains plating solution C, color becomes light blue by navy blue.?
The methanol of 2ml is added in the C liquid of 100ml, obtains D liquid.Plating solution E is obtained until pH=9 with the pH value that NaOH solution adjusts D liquid.
(6) to step (4) resulting nano-aluminum nitridenpE liquid is added according to 5g:40ml in particle, and sonic oscillation 30min is being stirred
In the case where, formaldehyde is added dropwise, wherein the ratio of suspension and formaldehyde is 40ml:2.5ml, is then adjusted with the NaOH solution prepared
PH value is between 11~12.After complete reaction, particle centrifuge washing is coated into nano-aluminum nitride to required CunpParticle.
(7) Cu for obtaining step (6) coats nano-aluminum nitridenpParticle and 7075 Al alloy powders are in the ambiance of argon gas
Carry out high-energy ball milling mixing, ratio of grinding media to material control is 5 ~ 10:1, and ball milling speed control is 150 ~ 350rmp, the control of ball time rate for 2 ~
5h.Cold welding occurs between particle and ball grinder in order to prevent, 1vol% stabilizer stearic acid is added in mixed-powder, will mix
Powder pressure maintaining 10min at 400MPa by cold pressing is prepared into Cu cladding nano-aluminum nitridenp/ 7075 prefabricated sections.
(8) prefabricated section that step (7) obtains is put into graphite jig, to guarantee the higher densification of blank in hot pressing
Degree, carries out vacuum heating-press sintering under mushy zone (between the solidus and liquidus temperature of 7075 aluminium alloys) for powder compact,
Sintering temperature control is 480 ~ 590 DEG C, and axial compressive force control is 20 ~ 50MPa, and heating rate control is 10 DEG C/min, vacuum degree
It is maintained at 3 × 10-5MPa keeps the temperature 10min when temperature reaches 250 DEG C, to guarantee to remove stearic acid.After reaching sintering temperature, protect
Warm time control is 60 ~ 120min, then obtains product blank.
(9) gained blank is subjected to plasticity thermal deformation field and reduces defect and Broken Crystal and Mg to reach17Al12Altogether
Crystal phase effect, extrusion ratio control are 16 ~ 42, and extruding rate control is 1 ~ 10mm/min, and temperature control is 350 ~ 500 DEG C.
(10) gained club-shaped material carries out Equal Channel Angular Pressing processing again, and temperature control is 150 ~ 200 DEG C, and angle control is
110 ~ 160 °, extrusion passes control is 5 ~ 7 times, and extruding rate control is 1 ~ 10mm/min.
The present invention is coated on nano aluminum nitride core surface using metallic copper, with improve nano aluminum nitride and 7075 matrixes it
Between interface bond strength, and coat nano-aluminum nitride by introducing vacuum hotpressing come quantitative addition high-content CunpThe composite wood of particle
Material, wherein the content of copper clad nano aluminum nitride is 2.5wt% ~ 6.5wt%.
The present invention has following uniqueness: (1) making the reinforced phase in composite material using high-energy ball milling and vacuum hotpressing
It is evenly dispersed.(2) the method reduce reinforced phase particle scaling loss, the increasing for the addition higher amount that can be quantified to a certain extent
Strong phase particle.(3) nano-aluminum nitride in coatingnpDue to there is the protective effect of Cu, while there is more preferable interface, increase and gold
The wetability of category, further reduces nano-aluminum nitridenpReunion probability.(4) it is forced during plasticity thermal deformation field using shearing
Broken grain grain, and cause dislocation to tangle and provide driving force for the dynamic recrystallization of composite material, achieve the purpose that refine crystal grain.(5)
Reinforced phase and interphase can effectively be dispersed again during carrying out Equal Channel Angular Pressing processing, to improve the machinery of product
Performance.
Specific embodiment
The present invention will be described further by following embodiment.
Embodiment 1.
By nano-aluminum nitridenpBe placed in 10%NaOH solution boil keep 30min, filter off NaOH solution deionized water to
Grain constantly flushing is in neutrality up to pH value, filtering drying.Above-mentioned particle is put into concentrated hydrochloric acid and is boiled 30 minutes, is carried out at roughening
Reason, is then cleaned with deionized water, is dried.Under mechanical stirring, by the SnCl of 10g22H2O is dissolved in 20ml hydrochloric acid, then uses
The dilution of 100ml distilled water, then adds the NaCl of 25g, obtains sensitizing solution after waiting solids to be completely dissolved.Then particle is placed in
Mechanical stirring 10min in sensitizing solution.By the PdCl of 1g2It is added in 100ml distilled water, waits after being completely dissolved, be added while stirring
50ml hydrochloric acid, stirring obtain activating solution until transparent.It is added to the particle being sensitized into activating solution, stirs 10min, later
It stands.After powder precipitating, filtering, then powder is washed with deionized.10gCuSO4•5H2O is dissolved in about 100ml distilled water
In, stirring and dissolving obtains clear blue solution A.60g sodium potassium tartrate tetrahydrate is dissolved in 100ml distilled water, stirring and dissolving obtains
To colourless clear solution B.In the case of stirring, B liquid is poured into A liquid and obtains plating solution C, color becomes light blue by navy blue
Color.The methanol of 2ml is added in 100mlC liquid, obtains D liquid.It is plated with the pH value that NaOH solution adjusts D liquid until pH=9
Liquid E.To the 5g nano-aluminum nitride after sensitization plays and activationnp40mlE liquid, sonic oscillation 30min, the case where stirring is added in particle
Under, 2.5ml formaldehyde is added dropwise to obtained 40ml suspension, then adjusts pH value between 11~12 with the NaOH solution prepared.
After complete reaction, particle centrifuge washing is obtained into required Cu and coats nano-aluminum nitridenpParticle.
Cu is coated into nano-aluminum nitridenpParticle carries out high-energy ball milling with 7075 Al alloy powders in the ambiance of argon gas and mixes,
Cu coats nano-aluminum nitridenpGranule content control is 2.5wt%, and ratio of grinding media to material control is 5:1, and ball milling speed control is 150rmp, when ball
Between rate control be 2h.Cold welding occurs between particle and ball grinder in order to prevent, it is stearic that 1vol% stabilizer is added in mixed-powder
Acid is prepared into Cu cladding nano-aluminum nitride by mixed-powder by being cold-pressed the pressure maintaining 10min at 400MPanp/ 7075 prefabricated sections.It will be pre-
Clamp dog is put into graphite jig, carries out vacuum heating-press sintering, and sintering temperature control is 480 DEG C, and axial compressive force control is 20MPa,
Heating rate control is 10 DEG C/min, and vacuum degree is maintained at 3 × 10-5MPa keeps the temperature 10min when temperature reaches 250 DEG C, to protect
Card removes stearic acid.After reaching sintering temperature, soaking time control is 60min, and subsequent arrives blank.Gained blank is moulded
Property thermal deformation field to reach reduce defect and Broken Crystal and Mg17Al12Eutectic phase separation, extrusion ratio control are 16, are squeezed
Rate control is 1mm/min, and temperature control is 350 DEG C.Gained club-shaped material carries out Equal Channel Angular Pressing processing, temperature control again
It is 150 DEG C, angle control is 110 °, and extrusion passes control is 5 times, and extruding rate control is 1mm/min, ultimate tensile strength
14.37% is improved compared with matrix.
Embodiment 2.
By nano-aluminum nitridenpBe placed in 10%NaOH solution boil keep 30min, filter off NaOH solution deionized water to
Grain constantly flushing is in neutrality up to pH value, filtering drying.Above-mentioned particle is put into concentrated hydrochloric acid and is boiled 30 minutes, is carried out at roughening
Reason, is then cleaned with deionized water, is dried.Under mechanical stirring, by the SnCl of 10g22H2O is dissolved in 20ml hydrochloric acid, then uses
The dilution of 100ml distilled water, then adds the NaCl of 25g, obtains sensitizing solution after waiting solids to be completely dissolved.Then particle is placed in
Mechanical stirring 10min in sensitizing solution.By the PdCl of 1g2It is added in 100ml distilled water, waits after being completely dissolved, be added while stirring
50ml hydrochloric acid, stirring obtain activating solution until transparent.It is added to the particle being sensitized into activating solution, stirs 10min, later
It stands.After powder precipitating, filtering, then powder is washed with deionized.10gCuSO4•5H2O is dissolved in about 90ml distilled water,
Stirring and dissolving obtains clear blue solution A.60g sodium potassium tartrate tetrahydrate is dissolved in 100ml distilled water, stirring and dissolving obtains nothing
The clear solution B of color.In the case of stirring, B liquid is poured into A liquid and obtains plating solution C, color becomes light blue by navy blue.
The methanol of 2ml is added in 100mlC liquid, obtains D liquid.Plating solution E is obtained until pH=9 with the pH value that NaOH solution adjusts D liquid.
To the 5g nano-aluminum nitride after sensitization plays and activationnpParticle addition 40mlE liquid, sonic oscillation 30min, in the case of stirring, to
2.5ml formaldehyde is added dropwise in obtained 40ml suspension, then adjusts pH value between 11~12 with the NaOH solution prepared.Wait react
After completely, particle centrifuge washing is obtained into required Cu and coats nano-aluminum nitridenpParticle.
Cu is coated into nano-aluminum nitridenpParticle carries out high-energy ball milling with 7075 Al alloy powders in the ambiance of argon gas and mixes,
Cu coats nano-aluminum nitridenpGranule content control is 4.5wt%, and ratio of grinding media to material control is 10:1, and ball milling speed control is 250rmp, when ball
Between rate control be 4h.Cold welding occurs between particle and ball grinder in order to prevent, it is stearic that 1vol% stabilizer is added in mixed-powder
Acid is prepared into Cu cladding nano-aluminum nitride by mixed-powder by being cold-pressed the pressure maintaining 10min at 400MPanp/ 7075 prefabricated sections.It will be pre-
Clamp dog is put into graphite jig, carries out vacuum heating-press sintering, and sintering temperature control is 550 DEG C, and axial compressive force control is 35MPa,
Heating rate control is 10 DEG C/min, and vacuum degree is maintained at 3 × 10-5MPa keeps the temperature 10min when temperature reaches 250 DEG C, to protect
Card removes stearic acid.After reaching sintering temperature, soaking time control is 90min, and subsequent arrives blank.Gained blank is moulded
Property thermal deformation field to reach reduce defect and Broken Crystal and Mg17Al12Eutectic phase separation, extrusion ratio control are 42, are squeezed
Rate control is 10mm/min, and temperature control is 350 DEG C.Gained club-shaped material carries out Equal Channel Angular Pressing processing, temperature control again
250 DEG C are made as, angle control is 160 °, and extrusion passes control is 7 times, and extruding rate control is 10mm/min, Ultimate Tensile
Intensity improves 18.31% compared with matrix.
Embodiment 3.
By nano-aluminum nitridenpBe placed in 10%NaOH solution boil keep 30min, filter off NaOH solution deionized water to
Grain constantly flushing is in neutrality up to pH value, filtering drying.Above-mentioned particle is put into concentrated hydrochloric acid and is boiled 30 minutes, is carried out at roughening
Reason, is then cleaned with deionized water, is dried.Under mechanical stirring, by the SnCl of 10g22H2O is dissolved in 20ml hydrochloric acid, then uses
The dilution of 100ml distilled water, then adds the NaCl of 25g, obtains sensitizing solution after waiting solids to be completely dissolved.Then particle is placed in
Mechanical stirring 10min in sensitizing solution.By the PdCl of 1g2It is added in 100ml distilled water, waits after being completely dissolved, be added while stirring
50ml hydrochloric acid, stirring obtain activating solution until transparent.It is added to the particle being sensitized into activating solution, stirs 10min, later
It stands.After powder precipitating, filtering, then powder is washed with deionized.10gCuSO4•5H2O is dissolved in about 100ml distilled water
In, stirring and dissolving obtains clear blue solution A.60g sodium potassium tartrate tetrahydrate is dissolved in 100ml distilled water, stirring and dissolving obtains
To colourless clear solution B.In the case of stirring, B liquid is poured into A liquid and obtains plating solution C, color becomes light blue by navy blue
Color.The methanol of 2ml is added in 100mlC liquid, obtains D liquid.It is plated with the pH value that NaOH solution adjusts D liquid until pH=9
Liquid E.To the 5g nano-aluminum nitride after sensitization plays and activationnp40mlE liquid, sonic oscillation 30min, the case where stirring is added in particle
Under, 2.5ml formaldehyde is added dropwise to obtained 40ml suspension, then adjusts pH value between 11~12 with the NaOH solution prepared.
After complete reaction, particle centrifuge washing is obtained into required Cu and coats nano-aluminum nitridenpParticle.
Cu is coated into nano-aluminum nitridenpParticle carries out high-energy ball milling with 7075 Al alloy powders in the ambiance of argon gas and mixes,
Cu coats nano-aluminum nitridenpGranule content control is 6.5wt%, and ratio of grinding media to material control is 5:1, and ball milling speed control is 350rmp, when ball
Between rate control be 5h.Cold welding occurs between particle and ball grinder in order to prevent, it is stearic that 1vol% stabilizer is added in mixed-powder
Acid is prepared into Cu cladding nano-aluminum nitride by mixed-powder by being cold-pressed the pressure maintaining 10min at 400MPanp/ 7075 prefabricated sections.It will be pre-
Clamp dog is put into graphite jig, carries out vacuum heating-press sintering, and sintering temperature control is 590 DEG C, and axial compressive force control is 50MPa,
Heating rate control is 10 DEG C/min, and vacuum degree is maintained at 3 × 10-5MPa keeps the temperature 10min when temperature reaches 250 DEG C, to protect
Card removes stearic acid.After reaching sintering temperature, soaking time control is 120min, and subsequent arrives blank.Gained blank is carried out
Plasticity thermal deformation field reduces defect and Broken Crystal and Mg to reach17Al12Eutectic phase separation, extrusion ratio control are 42, are squeezed
Pressure rate control is 10mm/min, and temperature control is 500 DEG C.Gained club-shaped material carries out Equal Channel Angular Pressing processing, temperature again
Control is 250 DEG C, and angle control is 110 °, and extrusion passes control is 7 times, and extruding rate control is 10mm/min, and the limit is anti-
Tensile strength improves 16.24% compared with matrix.
Claims (1)
1. a kind of nano aluminum nitride enhances the hot-press method of 7075 aluminium alloys, it is characterized in that the following steps are included:
(1) by nano-aluminum nitridenpBe placed in 10%NaOH solution boil keep 30min, filter off NaOH solution, with deionized water to
Grain constantly flushing is in neutrality up to pH value, filtering drying；
(2) particle in step (1) is put into concentrated hydrochloric acid and is boiled 30 minutes, carry out roughening treatment, it is then clear with deionized water
It washes, dries；
(3) step (2) obtained particle is placed in mechanical stirring 10min in sensitizing solution, wherein sensitizing solution proportion is SnCl2•
2H2O:HCl:NaCl:H2O=10g:20ml:25g:100g；
(4) activating solution is added in the particle in step (3), stirs 10min, stands later, and wherein the proportion of activating solution is PdCl2:
Hydrochloric acid: H2O=1g:50ml:100g；After powder precipitating, filtering, then powder is washed with deionized；
(5) in the ratio of 10g:90~100ml, by CuSO4•5H2O is dissolved in distilled water, stirring and dissolving, obtains clear blue
Solution A；In the ratio of 60g:100ml, sodium potassium tartrate tetrahydrate is dissolved in distilled water, stirring and dissolving, obtains colourless clear solution
B；In the case of stirring, the B liquid of equivalent is poured into A liquid and obtains plating solution C, color becomes light blue by navy blue；In 100ml
C liquid in be added 2ml methanol, obtain D liquid；Plating solution E is obtained until pH=9 with the pH value that NaOH solution adjusts D liquid；
(6) to step (4) resulting nano-aluminum nitridenpE liquid, sonic oscillation 30min, in the feelings of stirring is added according to 5g:40ml in particle
Under condition, formaldehyde is added dropwise, wherein the ratio of suspension and formaldehyde is 40ml:2.5ml, then adjusts pH value with the NaOH solution prepared
Between 11~12；After complete reaction, particle centrifuge washing is coated into nano-aluminum nitride to required CunpParticle；
(7) Cu for obtaining step (6) coats nano-aluminum nitridenpParticle carries out in the ambiance of argon gas with 7075 Al alloy powders
High-energy ball milling mixing, ratio of grinding media to material control are 5 ~ 10:1, and ball milling speed control is 150 ~ 350rmp, and the control of ball time rate is 2 ~ 5h；
1vol% stabilizer stearic acid is added in mixed-powder, by the mixed-powder pressure maintaining 10min at 400MPa, preparation by cold pressing
Nano-aluminum nitride is coated at Cunp/ 7075 prefabricated sections；
(8) prefabricated section that step (7) obtains is put into graphite jig, to guarantee the higher consistency of blank in hot pressing,
Powder compact is subjected to vacuum heating-press sintering between the solidus and liquidus temperature of 7075 aluminium alloys, sintering temperature control is
480 ~ 590 DEG C, axial compressive force control is 20 ~ 50MPa, and heating rate control is 10 DEG C/min, and vacuum degree is maintained at 3 × 10- 5MPa keeps the temperature 10min when temperature reaches 250 DEG C；After reaching sintering temperature, soaking time control is 60 ~ 120min, obtains base
Material；
(9) gained blank is subjected to plasticity thermal deformation field, extrusion ratio control is 16 ~ 42, and extruding rate control is 1 ~ 10mm/
Min, temperature control are 350 ~ 500 DEG C；
(10) gained club-shaped material carries out Equal Channel Angular Pressing processing again, and temperature control is 150 ~ 200 DEG C, angle control for 110 ~
160 °, extrusion passes control is 5 ~ 7 times, and extruding rate control is 1 ~ 10mm/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115261660A (en) * | 2022-09-30 | 2022-11-01 | 昆明理工大学 | Preparation method of high-strength high-heat-conductivity aluminum alloy material |
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| CN115261660B (en) * | 2022-09-30 | 2022-12-20 | 昆明理工大学 | Preparation method of high-strength high-heat-conductivity aluminum alloy material |
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