CN109402449A - A kind of Zn-TiB2The preparation method of efficiently rotten intermediate alloy and silk - Google Patents

A kind of Zn-TiB2The preparation method of efficiently rotten intermediate alloy and silk Download PDF

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CN109402449A
CN109402449A CN201811643009.9A CN201811643009A CN109402449A CN 109402449 A CN109402449 A CN 109402449A CN 201811643009 A CN201811643009 A CN 201811643009A CN 109402449 A CN109402449 A CN 109402449A
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tib
intermediate alloy
silk
powder
rotten
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CN109402449B (en
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张金山
赵锐
张佳欣
许春香
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Taiyuan University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C18/00—Alloys based on zinc
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • 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
    • C22C32/0073—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 borides

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Conductive Materials (AREA)

Abstract

A kind of Zn-TiB2The preparation method of efficiently rotten intermediate alloy and silk, is used for magnesium-zinc system and magnesium-zincium-rare earth system alloy modification micronization processes.The mass percent of the intermediate alloy raw material is: the TiB of the Zn of 80%-60%, 20-40%2, inevitable impurity.The preparation method of the intermediate alloy silk is by micron order Zn powder, nanoscale TiB2With additives dry blended ball milling, briquetting, be squeezed into silk.Intermediate alloy silk of the present invention carries out playing the role of refinement and regulation crystal growth pattern with instantaneous Metamorphism treatment is flowed, improving mechanical property and plastic deformation ability when can be used in semicontinuous casting rod and the production of continuous casting and rolling plate.The performance of alloy through being obtained after rotten with this silk improves toughness while improving intensity.

Description

A kind of Zn-TiB2The preparation method of efficiently rotten intermediate alloy and silk
Technical field
The invention belongs to metal material and molding field, in particular to a kind of Zn-TiB2Efficiently rotten intermediate alloy and silk Preparation method.When being produced for magnesium-Zn based alloy or magnesium-semicontinuous casting rod of zincium-rare earth system alloy and continuous casting and rolling plate into Row plays the role of refinement and regulation crystal growth pattern, improves mechanical property and plastic deformation ability with stream Metamorphism treatment.
Background technique
Magnesium alloy is known as the green engineering structural material of this century resource and environment sustainable development, magnesium-zincium-rare earth system Wrought magnesium alloy has a wide range of applications potentiality and development space in Aeronautics and Astronautics, the vehicles.In recent years, in magnesium-zinc- Have found that a kind of novel long period stacking order structure phase, the structure can mutually improve magnesium alloy strength in rare earth-based alloy It is smaller on plasticity influence simultaneously, and there is good thermodynamic stability at high temperature.By the length in magnesium-zincium-rare earth system alloy Period stacking order structure causes the extensive concern of domestic and international investigation of materials person as a kind of novel reinforced phase, becomes Magnesium alloy strengthens and the hot spot of preparation research.
But the crystal structure and slip system of magnesium alloy close-packed hexagonal determine that its plastic deformation ability is poor less, serious shadow Ring the working ability of magnesium alloy.And theory and practice proves, the plasticity that tiny equiaxial grain structure can improve magnesium alloy becomes Shape ability.In addition it also found when to magnesium-zincium-rare earth system superhigh strength magnesium alloy preparation research, to containing long-periodic structure If mutually magnesium-zincium-rare earth system alloy of enhancing is without especially handling during crystallization and freezing, primary α-Mg and the phase of precipitation (ten W of 18R) if grown and grown up in a manner of coupled growth, not only coarse grains, and crystal growth after solidification High directivity, finally makes that the intensity of alloy is low, brittleness is big, and hardly possible deformation prevents the performance advantage of this magnesium alloy from showing, applies It is restricted.W is MgZnY compound phase.
And Metamorphism treatment can not only significant refining alloy tissue, improve the mechanical property of magnesium alloy, improve casting character, subtract The casting flaws such as few hot tearing, loose.And magnesium alloy crystal grain is more tiny, and plastic deformation ability is better.In addition, by Metamorphism treatment Intermetallic compound phase afterwards in alloy is more tiny and is more evenly distributed, so as to shorten before plastic processing Homogenization Treatments when Between, Homogenization Treatments effect is improved, plastic deformation ability is improved.So especially heavy to magnesium-zincium-rare earth system alloy Metamorphism treatment It wants.
For this purpose, if a kind of Zn-TiB can be prepared2Intermediate alloy silk, to pour magnesium-zincium-rare earth series deformation magnesium alloy melt It infuses and is carried out in process of setting with instantaneous Metamorphism treatment is flowed, this is to magnesium-semicontinuous casting rod of zincium-rare earth series deformation magnesium alloy, continuous casting It even squeezes pole stock or the production of continuous casting and rolling plate and structure property regulation has great importance.
Summary of the invention
In order to improve the mechanical property of magnesium alloy, improves casting character, reduce the casting flaws such as hot tearing, loose, the present invention A kind of Zn-TiB is provided2The preparation method of efficiently rotten intermediate alloy and silk.
A kind of technical solution of the present invention: Zn-TiB2Efficiently rotten intermediate alloy, it is characterized in that material quality percentage It is: the TiB of the Zn of 80%-60%, 20-40%2, inevitable impurity.
A kind of Zn-TiB2The preparation method of efficiently rotten intermediate alloy, the raw material is mixed with additive, described to add Agent is added to account for the 0.2%-1.0% of material quality, under inert gas protection through ball mill ball milling 1-2 hours；Then it presses in a mold Power is the prefabricated section that the constant pressure lower lock block of 25-35MPa is 45-55% at relative density, and prefabricated section is put into chamber type electric resistance furnace 300-400 DEG C is taken out after heat preservation 1-2 hours.
A kind of Zn-TiB2The preparation method of efficiently rotten intermediate alloy silk, it is characterised in that the Zn-TiB2Efficiently become Matter intermediate alloy, which is put into extruder mold, is squeezed into Zn-TiB under 25-35MPa pressure2Efficiently rotten intermediate alloy silk.
Intermediate alloy silk of the invention can not only make magnesium-zincium-rare earth system alloy modification refinement, but also can make magnesium- The further Strengthening and Toughening of mechanical property of zincium-rare earth system alloy.When semicontinuous casting rod and continuous casting and rolling plate production when will be this It is molten that intermediate alloy silk can not only save Melting Magnesium-zincium-rare earth system alloy mother liquor when being added in a manner of going bad with stream instant inoculation Special zincification process when body, can also save alloy wire dosage, improve modifying-refining effect, Effective Regulation Solidification Structure, Mechanical property and plastic deformation processing performance.The present invention improves magnesium-Zn based alloy or magnesium-zincium-rare earth system alloy casting state toughness 23%, after extrusion deformation magnesium-Zn based alloy or magnesium-zincium-rare earth system alloy ductility improve 33%.
Detailed description of the invention
Fig. 1 is Zn-TiB prepared by the embodiment of the present invention 12Intermediate alloy silk scanning electron microscope microstructure picture.
Fig. 2 is Zn-TiB prepared by the embodiment of the present invention 12The metallograph of intermediate alloy ingot casting as-cast structure.
Fig. 3 is Zn-TiB prepared by the embodiment of the present invention 22Intermediate alloy silk scanning electron microscope microstructure picture.
Fig. 4 is Zn-TiB prepared by the embodiment of the present invention 22The metallograph of intermediate alloy ingot casting as-cast structure.
Fig. 5 is Zn-TiB prepared by the embodiment of the present invention 32Intermediate alloy silk scanning electron microscope microstructure picture.
Fig. 6 is Zn-TiB prepared by the embodiment of the present invention 32The metallograph of intermediate alloy ingot casting as-cast structure.
Specific embodiment
Embodiment 1:
(1) 80%Zn, 20%TiB by mass percentage2Additives ratio ingredient with raw material quality 0.2% is accounted for, weighs required Nanometer TiB2Powder and micron order zinc powder, under protection of argon gas through ball mill ball milling 1 hour；
(2) being hot pressed into relative density after preheating powder after mixing 1 hour under 25MPa pressure in a mold is 45% Prefabricated section；
(3) prefabricated section is placed in the chamber type electric resistance furnace of blanketing with inert gas, keeps the temperature 1 hour at 300 DEG C；
(4) prefabricated section for taking out preheated heat preservation, is put into extruder mold and is squeezed into silk under 25MPa pressure, be prepared into Zn- TiB2Intermediate alloy silk, microscopic structure are by η-Zn+TiB2Particle two-phase is formed, scanning electron microscope microstructure picture such as Fig. 1 It is shown.
(5) by the Zn-TiB of mass ratio 1.0%2Intermediate alloy silk is added in Mg-2.5Zn-2.5Y magnesium alloy, obtains after solidification The ingot casting as-cast structure obtained is made of α-Mg+W+18R three-phase, and metallographic structure is as shown in Fig. 2, as cast condition mechanical property σ b =289MPa, elongation δ=19%.
Embodiment two:
(1) 70%Zn, 30%TiB by mass percentage2With the additives ratio ingredient for accounting for raw material quality 0.6%, weigh required Nanometer TiB2Powder, micron order zinc powder and additive powder, under protection of argon gas through ball mill ball milling 1.5 hours；
(2) being hot pressed into relative density in a mold after preheating powder after mixing 1.5 hours under 30MPa pressure is 50% prefabricated section；
(3) prefabricated section is placed in the chamber type electric resistance furnace of blanketing with inert gas, keeps the temperature 1.5 hours at 350 DEG C；
(4) prefabricated section for taking out preheated heat preservation, is put into extruder mold and is squeezed into silk under 30MPa pressure, be prepared into Zn- TiB2Intermediate alloy silk, microscopic structure are by η-Zn+TiB2Particle two-phase is formed, scanning electron microscope microstructure picture such as Fig. 3 It is shown
(5) by the Zn-TiB of mass ratio 2.5%2Intermediate alloy silk is added in Mg-2.5Zn-2.5Y magnesium alloy, obtains after solidification Ingot casting as-cast structure is made of α-Mg+W+18R three-phase, metallographic structure as shown in figure 4, its as cast condition mechanical property σ b= 295MPa, elongation δ=18%.
Embodiment 3:
(1) 60% micron order Zn powder by mass percentage, 40%TiB2Nano powder and the additives ratio for accounting for raw material quality 1.0% Ingredient, nanometer TiB required for weighing2Powder, zinc powder and additive powder, under protection of argon gas through ball mill ball milling 2 hours；
(2) being hot pressed into relative density in a mold after preheating powder after mixing 2.0 hours under 40MPa pressure is 55% prefabricated section；
(3) prefabricated section is placed in the chamber type electric resistance furnace of blanketing with inert gas, keeps the temperature 2 hours at 400 DEG C；
(4) prefabricated section for taking out preheated heat preservation, is put into extruder mold and is squeezed into silk under 35MPa pressure, be prepared into Zn- TiB2Intermediate alloy silk, microscopic structure are by η-Zn+TiB2Particle two-phase is formed, scanning electron microscope microstructure picture such as Fig. 5 It is shown.
(5) by the Zn-TiB of mass ratio 1.5%2Intermediate alloy silk is added in Mg-2.5Zn-2.5Y magnesium alloy, obtains after solidification Ingot casting as-cast structure be made of α-Mg+W+18R three-phase, metallographic structure as shown in fig. 6, its as cast condition mechanical property σ b= 310MPa, elongation δ=23%.
Heretofore described additive uses potassium fluoborate.Contain inevitable impurity in zinc powder.

Claims (6)

1. a kind of Zn-TiB2Efficiently rotten intermediate alloy, it is characterized in that the mass percent of raw material is: the Zn of 80%-60%, 20- 40% TiB2, inevitable impurity.
2. a kind of Zn-TiB2The preparation method of efficiently rotten intermediate alloy, it is characterized in that by raw material described in claim 1 with add Agent is added to mix, the additive accounts for the 0.2%-1.0% of material quality, under inert gas protection through ball mill ball milling 1-2 hours； Then pressure is prefabricated section of the constant pressure lower lock block of 25-35MPa at relative density for 45-55% in a mold, and prefabricated section is put into Taking out after 300-400 DEG C of heat preservation 60-120min in chamber type electric resistance furnace is Zn-TiB2Efficiently rotten intermediate alloy.
3. a kind of Zn-TiB2The preparation method of efficiently rotten intermediate alloy silk, it is characterised in that by Zn- as claimed in claim 2 TiB2Intermediate alloy, which is put into extruder mold, is squeezed into Zn-TiB under 25-35MPa pressure2Intermediate alloy silk.
4. a kind of Zn-TiB2The preparation method of efficiently rotten intermediate alloy silk, it is characterised in that include the following steps:
(1) raw material by mass percentage 80% micron order zinc powder, 20% nanometer TiB2Powder；It adds again and accounts for raw material gross mass 0.2% additive, under protection of argon gas through ball mill ball milling mixing 1 hour, at uniform mixed powder；
(2) after preheating powder after mixing 1 hour under 25MPa pressure, being hot pressed into relative density in a mold is 45% Prefabricated section；
(3) prefabricated section is placed in the chamber type electric resistance furnace of blanketing with inert gas, in 300 DEG C of heat preservation 60min；
(4) prefabricated section for taking out preheated heat preservation, is put into extruder mold and is squeezed into silk under 25MPa pressure, be prepared into Zn- TiB2Intermediate alloy silk, microscopic structure are by η-Zn+TiB2Particle two-phase is formed；
(5) by the Zn-TiB of mass ratio 1.0%2Intermediate alloy silk is added in Mg-2.0Zn-2.0Y magnesium alloy fused mass, obtains after solidification The as-cast structure of ingot casting is made of α-Mg+W+18R three-phase, as cast condition mechanical property σ b=289MPa, elongation δ=19%.
5. a kind of magnesium-zincium-rare earth system alloy is with rotten crystal grain refinement Zn-TiB2The preparation method of intermediate alloy silk, feature exist In including the following steps:
(1) 70% micron order zinc powder by mass percentage, 30% TiB2Nano powder and the additive for accounting for raw material quality 0.6% Ingredient is carried out, under protection of argon gas through ball mill ball milling mixing 1.5 hours, at uniform mixed powder；
(2) by uniform mixed powder preheat 1.5 hours, apply 30MPa pressure be hot pressed into a mold relative density be 50% it is pre- Clamp dog；
(3) prefabricated section is placed in the chamber type electric resistance furnace of blanketing with inert gas, in 350 DEG C of heat preservation 90min；
(4) prefabricated section for taking out preheated heat preservation, is put into extruder mold and is squeezed into silk under 30MPa pressure, be prepared into Zn- TiB2Intermediate alloy silk；
(5) by the Zn-TiB of mass ratio 2.5%2Intermediate alloy silk is added in Mg-2.0Zn-2.0Y magnesium alloy fused mass, obtains after solidification The ingot casting as-cast structure obtained is made of α-Mg+W+18R three-phase, as cast condition mechanical property σ b=295MPa, elongation δ=18%.
6. a kind of Zn-TiB2The preparation method of efficiently rotten intermediate alloy silk, it is characterised in that include the following steps:
(1) raw material 60%Zn powder by mass percentage, 40%TiB2Nano powder；Account for the additives ratio of raw material quality 1.0% Ingredient, under protection of argon gas through ball mill ball milling 1 hour at uniform mixed powder；
(2) powder after mixing is preheated 2.0 hours and is hot pressed into relative density in a mold under 40MPa pressure and be 55% reaction prefabricated block；
(3) prefabricated section is placed in the chamber type electric resistance furnace of blanketing with inert gas, keeps the temperature 2 hours at 400 DEG C；
(4) prefabricated section for taking out preheated heat preservation, is put into extruder mold and is squeezed into silk under 35MPa pressure, be prepared into Zn- TiB2Intermediate alloy silk, microscopic structure are by η-Zn+TiB2Particle two-phase is formed；
(5) by the Zn-TiB of mass ratio 1.75%2Intermediate alloy silk is added in Mg-2.5Zn-2.5Y magnesium alloy, obtains after solidification Ingot casting as-cast structure is made of α-Mg+W+18R three-phase, as cast condition mechanical property σ b=310MPa, elongation δ=23%.
CN201811643009.9A 2018-12-29 2018-12-29 Zn-TiB2Preparation method of high-efficiency metamorphic intermediate alloy and wire Active CN109402449B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080060693A1 (en) * 2004-09-30 2008-03-13 Basf Aktiengesellschaft Thermoelectric Material Contact
CN104928511A (en) * 2015-06-30 2015-09-23 中南大学 Hot pressing sintering particle reinforcing zinc-based composite material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080060693A1 (en) * 2004-09-30 2008-03-13 Basf Aktiengesellschaft Thermoelectric Material Contact
CN104928511A (en) * 2015-06-30 2015-09-23 中南大学 Hot pressing sintering particle reinforcing zinc-based composite material and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
S. N. ALAM ET AL.: "Synthesis and Development of Zn-TiB2 Nanocomposites by Powder Metallurgy Route", 《MATERIALS TODAY: PROCEEDINGS》 *
YANBIN MA ET AL.: "Effect of TiB2-doping on the microstructure and mechanical properties of Mg-Zn-Y-Mn alloy", 《MATERIALS SCIENCE & ENGINEERING A》 *

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