CN110373565A - The preparation method of nano strengthened dispersion alloy - Google Patents
The preparation method of nano strengthened dispersion alloy Download PDFInfo
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- CN110373565A CN110373565A CN201910606305.XA CN201910606305A CN110373565A CN 110373565 A CN110373565 A CN 110373565A CN 201910606305 A CN201910606305 A CN 201910606305A CN 110373565 A CN110373565 A CN 110373565A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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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
- C22C1/10—Alloys containing non-metals
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- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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Abstract
The present invention relates to a kind of preparation methods of nano strengthened dispersion alloy, comprising the following steps: heats metal or alloy to be mixed, forms liquid metal or alloy melt；Nano particle is added to liquid metal or alloy melt in batches, is added every time with emulsification pretreatment dispersion is carried out with equipment, makes the nano particle being added in melt with acceleration GoptIt is mobile, and ultimately form mixed material dispersion suspension；Mixed material dispersion suspension is subjected to subsequent machining technology processing, nano dispersion reinforced metal or alloy is made；Preparation facilities includes mixing vessel, heating device, emulsifier unit, and emulsifier unit includes rotor and stator, and all side walls of stator are equipped with the gap passed through for melt.The preparation method and preparation facilities of nano strengthened dispersion alloy of the invention improve metal or alloy mechanical property and high temperature creep property, finally make the end properties produced stabilization, non-impurity-doped, at low cost, and be suitable for industrializing continuous production.
Description
Technical field
The present invention relates to field of material preparation, in particular to a kind of preparation method of nano strengthened dispersion alloy.
Background technique
Nano strengthened dispersion alloy material have excellent physical property and mechanical property, including room temperature intensity and high temperature it is strong
Degree, wearability, electric conductivity, thermal conductivity etc..It is tight by introducing stable, uniform, nanoscale particle and matrix in metallic matrix
Close combination, the nano particle pinning dislocation of Dispersed precipitate increase dislocation density, to enhance drawing hardening effect；In high temperature item
Under part, strengthen particle and do not dissolve and grow up, there is strong inhibition to dislocation motion and crystal boundary migration, reach anti-height
Warm softening power makes material have preferable mechanical behavior under high temperature, while the influence that particle scatters free electron is smaller,
Therefore the conductivity of metallic matrix will not be substantially reduced.
Currently, the preparation method of strengthened dispersion alloy mainly has mechanical alloying method, internal oxidation and chemical coprecipitation
Deng.
Published Chinese invention patent application 201710831279.1 prepares nano aluminium oxide using mechanical alloying method
Dispersion strengthening copper alloy.The Ball-milling Time that mechanical alloying method needs tens of or even hundreds of hours in large quantities of production, it is uncomfortable
Large-scale production is closed, long-time ball milling may cause coarse grains, and oxygen content is unable to control, and subsequent alloy is caused to densify
Disperse phase grows up and becomes submicron particles in technique, while more impurity can be introduced in mechanical milling process, not can avoid pollution,
It is had differences between batch end properties.
Published Chinese invention patent application 201210147029.3 prepares yttria dispersion strengthening using internal oxidation
Copper alloy.Internal oxidation process is difficult to control, and oxygen diffusion not exclusively may cause oxide and be unevenly distributed, complex process,
Period is long, and production cost is higher.
Published Chinese invention patent application 201810588877.5 prepares yttrium oxide disperse using chemical coprecipitation
Strengthen iron cobalt nickel alloy.The metal salt that chemical coprecipitation method is only limitted to all elements in material can be reacted with precipitating reagent,
The case where generating corresponding oxide or hydroxide precipitating, and process flow is longer, yield is lower, is suitable only for laboratory system
It is standby.
In addition to the preceding, the alloy material of conventional method preparation all has that nano particle addition difficulty is big, after addition
It is difficult to control it in the melt to reunite quickly and the problems such as melt separation, is difficult to obtain particle long period in alloy substrate
The state for keeping Dispersed precipitate not can guarantee quantitative addition and not can guarantee next with sufficiently long suspended stable state guarantee
The time requirement for walking processing, the alloy property after leading to forming are difficult to meet the needs of engineer application.
Summary of the invention
The purpose of the present invention is in order to solve the above problem, the present invention provides a kind of preparation side of nano strengthened dispersion alloy
Method.
According to an aspect of the present invention, a kind of preparation method of nano strengthened dispersion alloy is provided, comprising the following steps:
Metal or alloy to be mixed is heated, uniform liquid metal or alloy melt are formed；In batches by nano particle be added to
It in liquid metal or alloy melt, is added carries out high speed shearing emulsification dispersion with using equipment every time, make the nanometer being added
Particle is in melt with acceleration GoptIt is mobile, and ultimately form total mixed material dispersion suspension；Mixed material dispersion is outstanding
Turbid carries out subsequent machining technology processing, and nano strengthened dispersion alloy is made.
Wherein, the size of nano particle is 1-100nm；Acceleration of motion GoptFor 30-100G.
Wherein, in high speed shearing emulsification step, the addition batch of nano particle is more than or equal to 1 time, and every batch of addition is received
Rice grain and metal or alloy melt quality or volume ratio are 1:1000-1:100；The emulsification times of every batch of are 1-30min, often
The revolving speed for criticizing emulsifying device when being added is linear velocity 30-60m/s.
Wherein, metal or alloy is copper, aluminium, titanium, tin, copper alloy, aluminium alloy, titanium alloy, tin alloy or high temperature alloy
One of；Nano particle is graphene particles, carbon nanotube particulate, titanium dioxide granule, alumina particle, yttrium oxide, two
Silicon oxide particle, titanium carbide granule, silicon-carbide particle, aluminum nitride particle, boron nitride particle, tungsten carbide particle, boron particles, molybdenum
One of grain, cobalt granule, polyhedral polysilsesquioxane organic granular or polyhedral polysilsesquioxane composite particles are more
Kind.
Wherein, the nano particle total amount of addition and the volume or mass ratio of metal or alloy are 1:1000-1:10.
Wherein, the processing time of subsequent machining technology is 5-3600s.
Wherein, subsequent machining technology includes that mixed material atomization is made to the technique of metal or alloy powder or will be mixed
Alloy cube matherial is made in material cooling, the technique that bar, plate or band then is made in bulk.
According to known to research, during outer plus nano particle preparation nano strengthened dispersion alloy, the density one of particle
As with parent metal differ larger, and the two is mutually nonwetting, thus nano particle is easy to float in alloy melt, sink and group
It is poly-.Stokes particle drifts along speed υ expression formula are as follows:
υ=2gr2(ρMetal bath-ρNano particle)/9η
In formula, η is the viscosity (Pas) of molten metal；R is nano particle radius；G is acceleration of gravity；ρ is density.
According to above formula, the density contrast of drift along rate and nano particle and metal bath of the nano particle in metal bath and
Particle radius square is directly proportional, and is inversely proportional with the viscosity of metal bath.The viscosity for improving metal bath, reduces nano particle
Partial size can make the floating of particle or fall rate become smaller, to make particle dispersion mutually be not easy to assemble conglomeration, so that dispersion-strengtherning
The even tissue of alloy, performance boost.Under the premise of selected specific melt and nanometer additive, melt viscosity, melt and
The density of nano particle is definite value, drift along rate and the particle size of nano particle in the melt it is square directly proportional, therefore reduce
Nanoparticle size drift along to it separation of nano particle caused by rate and the influence grown up of reuniting it is maximum.
In the present invention, it ensure that bigger by high speed shearing emulsification technique using the opposite effect of high speed rotor and stator
Shearing force and higher shear velocity, so that nano particle is obtained high-strength acceleration Gopt, by micron order aggregate point
It is uniformly distributed from single nano particle, and in the melt, forms uniform suspension, on the other hand, realized to addition
Nano particle carries out broken dispersion repeatedly, and lasting shearing force minimizes the radius of particle, and then utmostly reduces matter
Speed of drifting along is put, so that metal bath-nano particle suspension is obtained the stable state of long period, makes subsequent technique
It completes, can guarantee in the metal or alloy product being eventually fabricated, nano particle is always within the retention time of the stable state
It is evenly dispersed state.Control to emulsification times, can make nano particle present in melt (including it is newest a batch be added
Nano particle) accelerated as much as possible, thus guarantee suspension and the metal or alloy product that finally obtains in, nanometer
Particle is more uniformly spread.
The preparation method of nano strengthened dispersion alloy of the invention is stirred by the emulsification of special parameter, is made into mixed
The sufficiently high acceleration of nanoparticle acquisition closed in material is moved, and then it is evenly dispersed to obtain nanoparticle, and is
Subsequent technique wins the enough processing time, improves metal or alloy mechanical property and high temperature creep property, finally makes
It is the end properties stabilization produced, non-impurity-doped, at low cost, and it is suitable for industrialization continuous production.
Detailed description of the invention
By reading the following detailed description of the preferred embodiment, various other advantages and benefits are common for this field
Technical staff will become clear.The drawings are only for the purpose of illustrating a preferred embodiment, and is not considered as to the present invention
Limitation.And throughout the drawings, the same reference numbers will be used to refer to the same parts.In the accompanying drawings:
Fig. 1 shows the flow chart of the preparation method of the nano strengthened dispersion alloy of embodiment according to the present invention.
Specific embodiment
The illustrative embodiments of the disclosure will be more fully described according to embodiment below.Although being shown in specification
The illustrative embodiments of the disclosure, it being understood, however, that may be realized in various forms the disclosure without that should be illustrated here
Embodiment limited.It is to be able to thoroughly understand the disclosure on the contrary, providing these embodiments, and can incite somebody to action
The scope of the present disclosure is fully disclosed to those skilled in the art.
As shown in Figure 1, the present invention provides a kind of preparation method of nano strengthened dispersion alloy, comprising the following steps: will be to
Mixed metal or alloy heating, forms it into uniform liquid metal or alloy melt；In batches by nano particle be added to
It in liquid metal or alloy melt, is added all carries out high shear agitation with using emulsifying device every time, so that is be added receives
The translational acceleration of rice grain reaches Gopt, until eventually forming evenly dispersed emulsification suspension；Suspension is subjected to subsequent add
Work process, is made nano strengthened dispersion alloy.
In above-mentioned steps, the size of the nano particle of addition is that 1-100nm is specifically as follows in some embodiments
1nm, 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm and 100nm.
In above-mentioned steps, high speed shearing emulsification disperses the final acceleration 30-100G for making mixed material, is specifically as follows
30G、40G、50G、60G、70G、80G、90G、100G。
In above-mentioned steps, the addition batch of nano particle is more than or equal to 1 time.In some embodiments, it is specifically as follows 1
Secondary, 2 times, 3 times, 4 times, 5 times, 6 times, 7 times, 8 times, 9 times, 10 times, the nano particle and metal or alloy melt matter of every batch of addition
Amount or volume ratio be 1:1000-1:200, in some specific embodiments, mass ratio can be 1:1000,1:800 |, 1:
600,1:400 or 1:200 or volume ratio can be 1:1000,1:800 |, 1:600,1:400 or 1:200；When every batch of is added
The revolving speed of emulsifying device is linear velocity 30-60m/s, according to Acceleration Formula a=v2The linear velocity of/r, the range can make particle
Obtain enough acceleration；Linear velocity when every batch of is added is specifically as follows 30m/s, 40m/s, 50m/s, 60m/s；The cream of every batch of
Change the time within 30min, is specifically as follows 20min, 25min, 30min.
In above-mentioned steps, the total addition level of nano particle and the quality of metal or alloy melt or volume ratio are 1:
1000-1:200, in some specific embodiments, volume ratio can for 1:1000,5:1000,1:100,2:100,3:100,
4:100,5:100,6:100,7:100,8:100,9:100,10:100；Quality accounting is specifically as follows 1:1000,5:1000,1:
100,2:100,3:100,4:100,5:100,6:100,7:100,8:100,9:100,10:100.
In above-mentioned steps, the processing time of processing technology is less than or equal to 1 hour, is specifically as follows 0.5h or 1h.
In above-mentioned steps, metal or alloy is copper, aluminium, titanium, tin, copper alloy, aluminium alloy, titanium alloy, tin alloy or height
One of temperature alloy；Nano particle is graphene particles, carbon nanotube particulate, titanium dioxide granule, alumina particle, dioxy
Silicon carbide particle, titanium carbide granule, silicon-carbide particle, aluminum nitride particle, boron nitride particle, tungsten carbide particle, boron particles, molybdenum
One of grain, cobalt granule, polyhedral polysilsesquioxane organic granular or polyhedral polysilsesquioxane composite particles are more
Kind.
Below by by way of specific embodiment, the preparation method of the application is described further.
Embodiment 1
3kg pure metal copper ingot is placed in graphite smelting furnace, is heated to 1200 DEG C under nitrogen atmosphere protection；It is complete to copper ingot
After running down, 3g nano alumina particles, particle size 100nm is added；By the emulsifying head of graphite high speed shearing emulsification dispersion machine
It protrudes into copper liquid, open and gradually rises revolving speed to linear velocity 60m/s；After the dispersion of 30min high speed shearing emulsification, it is added again
3g nano alumina particles, and high speed shearing emulsification 30min again repeat this process, until the accumulative 30g of addition altogether is nano oxidized
Alumina particles, and form nano alumina particles-copper melts suspension；Nano alumina particles-copper melts suspension is poured into mould
In tool, 20min is quickly cooled down using recirculated water, nano aluminum oxide dispersion is obtained and strengthens copper casting.
Copper casting is strengthened to nano aluminum oxide dispersion obtained, carries out distribution of particles detection and performance detection, the results show that
Nano aluminum oxide dispersion obtained is strengthened in copper casting, and the average headway of nano particle is 20 ± 5 μm, hardness HRB80, conductivity
90%IACS, tensile strength 580MPa, 900 DEG C of softening temperature.
Embodiment 2
2kg ferrochrome ingot (Fe-Cr12wt%) is placed in graphite smelting furnace, is heated under argon atmosphere protection
1500℃；After alloy pig is completely melt, 10g nano yttrium oxide particle, particle size 80nm is added；By graphite high speed shear cream
The emulsifying head for changing dispersion machine protrudes into tin liquor, opens and gradually rises revolving speed to linear velocity 40m/s；Through 20min high speed shear cream
After changing dispersion, nano yttrium oxide particle-ferrochrome melt suspension is poured into mold, is quickly cooled down using recirculated water
15min obtains nano yttrium oxide dispersion-strengtherning ferrochrome casting.
To nano yttrium oxide dispersion-strengtherning ferrochrome casting obtained, distribution of particles detection and performance detection, knot are carried out
Fruit shows, in nano yttrium oxide dispersion-strengtherning ferrochrome casting obtained, the spacing of nano particle is 13 ± 7 μm, and tension is strong
Spend 1580MPa, elongation after fracture 15.7%.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of the claim
Subject to enclosing.
Claims (7)
1. a kind of preparation method of nano strengthened dispersion alloy, which comprises the following steps:
Metal or alloy to be mixed is heated, uniform liquid metal or alloy melt are formed；
Nano particle is added into liquid metal or alloy melt in batches, is added carries out high speed with using equipment every time
Emulsification pretreatment dispersion makes the nano particle being added in melt with acceleration GoptIt is mobile, and ultimately form total mixed material point
Dissipate suspension；
Mixed material dispersion suspension is subjected to subsequent machining technology processing, nano strengthened dispersion alloy is made.
2. preparation method as described in claim 1, which is characterized in that
The size of nano particle is 1-100nm；Acceleration of motion GoptFor 30-100G.
3. preparation method as claimed in claim 2, which is characterized in that
In high speed shearing emulsification step, the addition batch of nano particle is the nano particle and gold of every batch of addition more than or equal to 1 time
Category or alloy melt quality or volume ratio are 1:1000-1:100；The emulsification times of every batch of are 1~30min, when every batch of is added
The revolving speed of emulsifying device is linear velocity 30-60m/s.
4. preparation method as described in claim 1, which is characterized in that
Metal or alloy is one of copper, aluminium, titanium, tin, copper alloy, aluminium alloy, titanium alloy, tin alloy or high temperature alloy；
Nano particle is graphene particles, carbon nanotube particulate, titanium dioxide granule, alumina particle, yttrium oxide, silica
Grain, titanium carbide granule, silicon-carbide particle, aluminum nitride particle, boron nitride particle, tungsten carbide particle, boron particles, molybdenum particle, cobalt
One of grain, polyhedral polysilsesquioxane organic granular or polyhedral polysilsesquioxane composite particles are a variety of.
5. preparation method as described in claim 1, which is characterized in that
The nano particle total amount of addition and the volume or mass ratio of metal or alloy are 1:1000-1:10.
6. preparation method as described in claim 1, which is characterized in that
The processing time of subsequent machining technology is 5~3600s.
7. preparation method as described in claim 1, which is characterized in that
Subsequent machining technology includes that the technique of metal or alloy powder is made in mixed material dispersion suspension atomization and will be mixed
It closes material cooling and alloy cube matherial, and the technique that bar, plate or band is made in bulk is made.
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| CN110744220A (en) * | 2019-11-15 | 2020-02-04 | 北京康普锡威科技有限公司 | Low-spatter welding wire and preparation method thereof |
| CN112853134A (en) * | 2020-12-31 | 2021-05-28 | 北京康普锡威科技有限公司 | Method for preparing alloy material by high-speed shearing and fine-grain alloy material obtained by same |
| CN114855017A (en) * | 2022-04-25 | 2022-08-05 | 合肥工业大学 | Y 2 O 3 CNT (carbon nanotube) -reinforced copper-based composite material and preparation method thereof |
| WO2023077881A1 (en) * | 2021-11-05 | 2023-05-11 | 中冶赛迪工程技术股份有限公司 | Nanoparticle-copper-iron composite alloy, and preparation and use thereof |
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| CN114855017A (en) * | 2022-04-25 | 2022-08-05 | 合肥工业大学 | Y 2 O 3 CNT (carbon nanotube) -reinforced copper-based composite material and preparation method thereof |
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