CN106244838A - Niobium titanium carbon Al-alloy alterant and preparation method thereof - Google Patents
Niobium titanium carbon Al-alloy alterant and preparation method thereof Download PDFInfo
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- CN106244838A CN106244838A CN201610836489.5A CN201610836489A CN106244838A CN 106244838 A CN106244838 A CN 106244838A CN 201610836489 A CN201610836489 A CN 201610836489A CN 106244838 A CN106244838 A CN 106244838A
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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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
Abstract
The invention discloses a kind of niobium titanium carbon Al-alloy alterant and preparation method thereof.Described niobium titanium carbon Al-alloy alterant is with niobium powder, titanium valve and graphite powder as raw material, and niobium, the mass ratio of titanium are 3:7～7:3, and carbon is 0.8:1～1:1 with the atomic ratio of niobium titanium.The preparation method of niobium titanium carbon Al-alloy alterant is first the mixed material ball milling of niobium powder, titanium valve to be become niobium titanium alloy, adds the further ball milling of graphite powder and makes carbon and the further alloying of niobium titanium alloy, and forms carbide nucleus.The niobium titanium carbon Al-alloy alterant of the present invention can notable refining aluminum alloy as-cast structure, improve the plasticity of cast aluminium alloy.
Description
Technical field
The invention belongs to material science, be specifically related to a kind of niobium titanium carbon Al-alloy alterant and preparation side thereof
Method.
Background technology
Aluminium alloy is one of metal material of application amount maximum, and its application amount is only below iron and steel.To metal material, tissue is thin
Change is to improve the strength of materials and plasticity most efficient method.Different from ferrous materials, aluminium alloy is not because having phase transformation, it is impossible to by heat
The mode thinning microstructure processed, can only pass through the means thinning microstructure such as Metamorphism treatment and thermal deformation.And Cast aluminium alloy is golden, rotten place
Reason just becomes unique thinning microstructure, improves the key technology means of cast properties, and is paid attention to widely.At Metamorphism treatment
In, alterant and technique have significant impact to structure refinement.At present, in Aluminum alloy modification, application preferably at most aluminum titanium boron,
Aluminum strontium alterant etc..Recently, the new alterant such as the carbide of compound rare-earth, the carbide of titanium, vanadium also begins to application.Alterant
Thinning microstructure it is crucial that can stable existence in the liquid phase, and interface can promote forming core as the core of heterogeneous forming core, carefully
Change tissue.Another factor affecting modification effect is rotten and casting technique.Conventional aluminum titanium boron alterant is to rate of cooling
The most sensitive, with the reduction of rate of cooling, the substantially roughening of its tissue, cause foundry goods different parts to produce substantially because thickness is different
Histological difference.Recent studies have shown that, use aluminum titanium carbon alterant also to have good effect.
Aluminum titanium carbon is to utilize titanium, carbon to form titanium carbide, and titanium, aluminum form aluminum Tritanium/Trititanium, and titanium carbide and aluminum Tritanium/Trititanium all can be made
For the core of aluminium alloy, growing up of suppression carbide, it is thus achieved that more tiny forming core points are effectively to utilize aluminum titanium carbon modification effect
Key.Niobium has the characteristic similar to titanium, it is also possible to form niobium carbide and aluminum three niobium, and titanium and niobium and be substituted for each other, and is formed
Titanium carbide niobium and aluminum Tritanium/Trititanium niobium.Additionally niobium has bigger atomic radius, and the diffusion in aluminum is more difficult, can effectively suppress carbide
And the roughening of aluminum Tritanium/Trititanium niobium, thus reduce because casting thickness is different, cause the different impact on modification effect of rate of cooling.Cause
This, preparing and obtain good modification effect niobium titanium carbon aluminum alloy modifier will become the key of refining aluminum alloy as-cast structure.
Summary of the invention
The technical issues that need to address of the present invention are to provide kind of a kind of niobium titanium carbon Al-alloy alterant and a preparation side thereof
Method, makes niobium, titanium, carbon have rational ratio and structure, plays good Aluminum alloy modification effect, refining aluminum alloy solidification group
Knit.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is: a kind of niobium titanium carbon Al-alloy goes bad
Agent, with niobium powder, titanium valve, graphite powder as raw material, described niobium powder, the mass ratio of titanium valve are 3:7～7:3；Graphite powder and niobium powder, titanium
The atomic ratio of powder is 0.8:1～1:1, and above-mentioned raw materials forms niobium titanium carbon composite powder through mechanical mill alloying, wherein comprises 70-
The carbide particle of the titanium carbide niobium of 80%.
The preparation method of a kind of niobium titanium carbon Al-alloy alterant, said method comprising the steps of:
Step A: be all higher than 98.0% with purity, its particle mean size niobium powder between 300 mesh～1000 mesh, titanium
Powder, graphite powder are raw material；
Step B: ball milling；
Step B1: the mixed material ball milling that mass ratio is 3:7～7:3 of niobium powder, titanium valve is become niobium titanium alloy powder body；
Step B2: add graphite powder in step B1 gained niobium titanium alloy powder body, described graphite powder and niobium powder, titanium valve former
Son ratio is 0.8:1～1:1, and under the protection of purity ＞ 99.99% of argon, further ball milling makes niobium titanium alloy be formed with graphite
Niobium titanium carbon composite powder, wherein comprises the carbide particle of the titanium carbide niobium of 70-80%.
Further improvement is that of the above-mentioned preparation method of the present invention: described ball milling step B1 is by niobium powder and certain proportion
Titanium valve mixing after load in ball grinder, the zirconium oxide balls in ball grinder is 15:1～40:1 with the mass ratio of material, ball milling
Tank is ball milling under the protection of purity ＞ 99.99% of argon, makes niobium powder form niobium titanium alloy powder body with titanium valve.
Owing to have employed technique scheme, the technological progress that the present invention obtains is:
This invention uses the method for mechanical alloying, makes niobium titanium be initially formed alloy, forms niobium titanium carbon with carbon more multiple
Close powder body, composite particles contains a certain amount of titanium carbide niobium nucleus, and due to the effect of mechanical alloying, niobium titanium carbon is combined
Granule exists a large amount of defect and high mechanical energy, when adding in high-temperature liquid state aluminium alloy, due to high temperature action, niobium, titanium,
Carbon energy fast reaction, on the basis of mechanical alloying forms carbide nucleus, generates tiny niobium carbide titanium, and is distributed to aluminum conjunction
In gold liquid.And a small amount of niobium, titanium, carbon dissolve in aluminum alloy melt during follow-up, effectively facilitate aluminium alloy along Carbide Precipitation and coagulate
Admittedly organize forming core, thinning solidification structure.
The first time mechanical milling process of the present invention achieve niobium powder, titanium valve broken, levigate, produce in making niobium, titanium granule simultaneously
The raw defect such as substantial amounts of room and dislocation, in the collision process of niobium powder and titanium valve, constantly refinement produces substantial amounts of unsalted surface
And the temperature rise of moment promotes niobium, Ti Alloying.
In the second time mechanical milling process of the present invention, mechanical alloying niobium titanium alloy powder and carbon dust are at mechanical mill energy
The lower diffusion to niobium titanium alloy accelerating carbon of effect, forms niobium titanium carbon composite powder, and under the effect of impact temperature, forms carbon
Compound nucleus, ultimately forms the aluminum alloy modifier of the niobium titanium carbon composite powder comprising certain carbide nucleus.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further details:
A kind of niobium titanium carbon Al-alloy alterant of the present invention is with niobium powder, titanium valve and graphite as raw material, described niobium powder,
The mass ratio of titanium valve is 3:7～7:3, and graphite powder is 0.8:1～1:1 with niobium powder, the atomic ratio of titanium valve total amount.This niobium titanium carbon is multiple
Close Aluminum alloy modification to be prepared by Mechanical Alloying.
Each embodiment balls grinding machine is the nanometer impact grinding that Qinhuangdao Tai Ji ring nanometer products company limited produces, ball
Grinding jar is stainless cylinder of steel, and volume is 2L, abrading-ball is also zirconium oxide material, has φ 10mm, the cumulative volume of abrading-ball accounts for the volume of tank
50%～70%.
Embodiment 1
The first step: (purity is 98.0%, granularity is by niobium powder (granularity be 1000 mesh, purity be 99.2%) and titanium valve
1000 mesh) press the mass ratio mixing of 3:7, load in stainless steel jar mill, and (zirconium oxide balls is with mixed according to the ratio of grinding media to material of 39:1
Close the mass ratio of powder) in grinding jar, load zirconia ball.It is filled with purity of argon to ball grinder > 99.99%, then rush in nanometer
Hit on mill, ball milling 1 hour under the rotating speed of 300r/min.
Second step: add the graphite powder (granularity identical with niobium powder and titanium valve atom summation in the ball grinder of the first step
Be 325 mesh, purity be 99.1%), be filled with purity > after the argon of 99.99%, under the rotating speed of 300r/min, continue ball milling 3 little
Time.
In the niobium titanium carbon Al-alloy alterant obtained, niobium, titanium mass ratio are 3:7.
Embodiment 2
The present embodiment is as follows with the difference of embodiment 1.
(granularity is that 1000 mesh, purity are for niobium powder used by the first step (granularity be 1000 mesh, purity be 99.2%) and titanium valve
98.0%) mixing for 1:1 in mass ratio, the zirconium oxide balls used is 30:1 with niobium powder, titanium valve mixed powder mass ratio, ball
Consume time 1.5 hours.
Second step adds graphite powder (granularity be 320 mesh, purity be 99.1%), graphite powder amount and niobium powder and titanium valve former
Son ratio is 0.9:1, and continuing Ball-milling Time is 3 hours.
In the niobium titanium carbon Al-alloy alterant obtained, niobium, titanium mass ratio are 1:1.
Embodiment 3
The present embodiment is as follows with the difference of embodiment 1.
(granularity is that 1000 mesh, purity are for niobium powder used by the first step (granularity be 1000 mesh, purity be 99.2%) and titanium valve
98.0%) pressing the mass ratio mixing of 7:3, the zirconium oxide balls used is 30:1 with niobium powder, titanium valve mixed powder mass ratio, ball
Consume time 1.5 hours.
Second step adds graphite powder (granularity be 320 mesh, purity be 99.1%), graphite powder amount and niobium powder and titanium valve former
Son ratio is 0.8:1, and continuing Ball-milling Time is 3.5 hours.
In the niobium titanium carbon Al-alloy alterant obtained, niobium, titanium mass ratio are 7:3.
Embodiment 4
The present embodiment is as follows with the difference of embodiment 1.
The granularity of first step niobium powder is 300 mesh, and purity is 98.0%, and the granularity of titanium valve is 320 mesh, and purity is 98.4%
Ball-milling Time is 2 hours.
The Ball-milling Time of second step is 4 hours.
In the niobium titanium carbon Al-alloy alterant obtained, niobium, titanium mass ratio are 3:7.
Embodiment 5
The present embodiment is as follows with the difference of embodiment 3.
The granularity of first step niobium powder is 300 mesh, and purity is 98.0%%, and the granularity of titanium valve is 320 mesh, and purity is 98.4%
Ball-milling Time be 2 hours.
The Ball-milling Time of second step is 4 hours.
Niobium, titanium mass ratio 7:3 in the niobium titanium carbon Al-alloy alterant obtained.
The result detecting above five embodiment gained samples is as follows:
First the powder body obtained by after terminating the first step carries out X-ray diffraction analysis, in the low embodiment of Ti content 1, in fact
Execute example 2 and implement in 4, thing equal niobium titanium alloy solid solution mutually；And in the high enforcement of Ti content 3 with implement in 5, thing is niobium titanium mutually
Solid solution and a small amount of titanium phase.Powder body obtained by after terminating second step carries out X-ray diffraction analysis, in X-ray diffraction spectrum
Do not find the diffraction maximum of carbon, in the low embodiment of Ti content 1, embodiment 2 and enforcement 4, thing equal niobium titanium carbon alloy solid solution mutually
And a small amount of niobium carbide titanium；With the increase of Ti content, in embodiment 2, embodiment 3, embodiment 4 and embodiment 5, niobium carbide titanium phase
Amount increased.
Embodiment 6
Prepared niobium titanium carbon Al-alloy alterant is applied to A356 aluminium alloy castings and with aluminum titanium boron alterant
Compare.Detailed description of the invention is as follows:
Being melted in middle hot-well formula soon by A356 aluminium alloy, fusion temperature is 690 DEG C ± 5 DEG C.Treat that aluminium alloy is completely melt also
After reaching 690 DEG C ± 5 DEG C, will be compared with aluminium alloy, above-described embodiment 1 that mass percent is 1.5% is obtained to embodiment 5
Niobium titanium carbon Al-alloy alterant add in aluminum liquid.Adding Way uses aluminium foil cladding, press-in and stirs, and adds and covers
Agent, logical argon is poured into a mould after giving vent to anger.Mold is the hot-die through 300 DEG C of preheatings.For silicon phase in refinement A356 aluminium alloy, it is simultaneously introduced matter
Amount is than the strontium alterant being 1%.For contrasting with aluminum titanium boron alterant, same process is used to be prepared for what aluminum titanium boron alterant went bad
Ingot casting, the addition mass percent that aluminum titanium boron goes bad is 2%.
Use the ingot material that above-described embodiment 1 is prepared to the niobium titanium carbon Al-alloy alterant that embodiment 5 is obtained
It is respectively labeled as A, B, C, D, E, and the ingot material using aluminum titanium boron alterant to prepare is labeled as F.
Cutting metallographic specimen and tensile property sample in the part that ingot casting is identical, under the microscope, the difference of measurement goes bad
After agent processes, ingot casting A, B, C, D, E, F aluminium alloy dendrite size is listed in the table below；Meanwhile, tensile yield strength and percentage elongation are also found in
Following table.
As can be seen here, under conditions of niobium titanium carbon alterant addition is less than aluminum titanium boron alterant, niobium titanium carbon alterant has
There is the modification effect suitable with aluminum titanium boron alterant.Niobium titanium carbon alterant when niobium titanium mass percent is 50:50, structure refinement
Best results.Using niobium titanium carbon alterant compared with the performance of aluminum titanium boron alterant ingot casting, niobium titanium carbon alterant makes casting strength
Slightly reduce, but plasticity dramatically increases.
Claims (3)
1. a niobium titanium carbon Al-alloy alterant, it is characterised in that: described alterant is former with niobium powder, titanium valve, graphite powder
Material, described niobium powder, the mass ratio of titanium valve are 3:7～7:3；Graphite powder is 0.8:1～1:1 with niobium powder, the atomic ratio of titanium valve, on
State raw material and form niobium titanium carbon composite powder through mechanical mill alloying, wherein comprise the carbide of the titanium carbide niobium of 70-80%
Grain.
2. the preparation method of a niobium titanium carbon Al-alloy alterant, it is characterised in that: said method comprising the steps of:
Step A: be all higher than 98.0% with purity, its particle mean size niobium powder between 300 mesh～1000 mesh, titanium valve, stone
Powdered ink is raw material；
Step B: ball milling；
Step B1: the mixed material ball milling that mass ratio is 3:7～7:3 of niobium powder, titanium valve is become niobium titanium alloy powder body；
Step B2: adding graphite powder in step B1 gained niobium titanium alloy, described graphite powder with the atomic ratio of niobium powder, titanium valve is
0.8:1～1:1, under the protection of purity ＞ 99.99% of argon, further ball milling makes niobium titanium alloy form niobium titanium carbon with graphite
Composite granule, wherein comprises the carbide particle of the titanium carbide niobium of 70-80%.
3. the preparation method of according to claim 2 niobium titanium carbon Al-alloy alterant, it is characterised in that: described ball milling
Step B1 be niobium powder is mixed with a certain proportion of titanium valve after load in ball grinder, the zirconium oxide balls in ball grinder and material
Mass ratio is 15:1～40:1, and ball grinder is ball milling under the protection of purity ＞ 99.99% of argon, makes niobium powder form niobium with titanium valve
Titanium alloy powder body.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114453567A (en) * | 2022-01-27 | 2022-05-10 | 江苏大学 | High-temperature alloy solidification structure refiner and preparation method and application thereof |
| CN114956822A (en) * | 2022-05-13 | 2022-08-30 | 咸阳职业技术学院 | Erosion-resistant corrosion-resistant high-temperature atomizing nozzle and preparation method thereof |
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| CN114453567A (en) * | 2022-01-27 | 2022-05-10 | 江苏大学 | High-temperature alloy solidification structure refiner and preparation method and application thereof |
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