CN105603230A - Method for preparing dispersed reinforced phase light Mg-Ti solid solution - Google Patents

Method for preparing dispersed reinforced phase light Mg-Ti solid solution Download PDF

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Publication number
CN105603230A
CN105603230A CN201610162567.8A CN201610162567A CN105603230A CN 105603230 A CN105603230 A CN 105603230A CN 201610162567 A CN201610162567 A CN 201610162567A CN 105603230 A CN105603230 A CN 105603230A
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ball
solid solution
nanometer
wild phase
preparing
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CN201610162567.8A
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Inventor
王辛
王章忠
孔凡新
吴梦陵
王鑫
杨启锐
李柏男
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Nanjing Institute of Technology
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Nanjing Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0408Light metal alloys
    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium

Abstract

The invention discloses a method for preparing a dispersed reinforced phase light Mg-Ti solid solution, belongs to the technical field of magnesium alloy matrix reinforcement and in particular relates to a method for preparing a dispersed phase reinforced matrix material with a similar crystal structure and properties. The preparation method is simple, production cost is low, the finished product Mg-Ti solid solution has excellent high temperature mechanical properties, the predicament that the Mg-Ti solid solution is difficult to produce by adopting the conventional casting method is effectively solved, densities of Mg and Ti elements are relatively low, the density of the Ti element is 4.54g/cm<3> only, and the formed Mg-Ti solid solution fully plays the light weight advantage of a magnesium alloy material; and Ti and Mg are of a close-packed hexagonal crystal structure, so that Ti and Mg have a good bonding interface, Ti element enters magnesium crystal lattices in a dispersed manner, and various performances of the solid solution are effectively improved.

Description

A kind of method of preparing disperse wild phase lightweight Mg-Ti solid solution
Technical field
The invention belongs to magnesium alloy substrate and strengthen technical field, particularly one has the increasing of phase quasi-crystalline structue disperse phaseThe method of strong matrix material structure and performance.
Background technology
Magnesium and magnesium alloy materials have that quality is light, specific strength is high, be easy to the advantages such as recycling, at Aeronautics and Astronautics, automobileThe fields such as manufacture, biomedicine all have a wide range of applications and development space. Then, magnesium and magnesium alloy materials have poorMechanical behavior under high temperature, this shortcoming makes it be difficult to meet under the relatively high environment of temperature and use, this is also to a certain degreeOn limited its application field, poor heat stability is restricting development and the application of magnesium and magnesium alloy materials always.
Various countries scholar and researcher have carried out various relevant experimental studies and have improved the high temperature of magnesium and magnesium alloy materialsPerformance for example, adds the method for rare metal to improve mechanical behavior under high temperature in magnesium and magnesium alloy substrate, adopts in this wayMain cause be that rare earth element has special configuration of extra-nuclear electron rule, this feature can make rare earth element at magnesium andIn magnesium alloy materials matrix, form the hardening constituent of disperse, the hardening constituent of disperse can improve its mechanical behavior under high temperature effectively. ThoughSo employing rare element can improve the mechanical behavior under high temperature of magnesium and magnesium alloy materials, but because the price of rare earth element is very highExpensive, production cost is high, is difficult to large-scale popularization and production, and this has limited to a certain extent rare earth and has strengthened magnesium and magnesium alloy materialApplication and the popularization of material.
Thereby, be badly in need of at present researching and developing a kind of novel disperse wild phase and improve the height of magnesium and magnesium alloy materialsTemperature mechanical property.
Summary of the invention
The object of the invention is that carrying out disperse for available technology adopting rare earth element strengthens magnesium and magnesium alloy materials processIn existing problem, provide one to utilize phase quasi-crystalline structue disperse phase to strengthen magnesium and magnesium alloy materials basal body structure and propertyThe method of energy.
In order to realize above-mentioned target, the present invention adopts following technical scheme:
A method of preparing disperse wild phase lightweight Mg-Ti solid solution, comprises the following steps:
S1, pure nanometer magnesium dust and the pure titanium powder of nanometer are carried out to proportioning by volume make composite material;
S2, by above-mentioned composite material and stainless steel abrading-ball proportioning in mass ratio, be sealed in ball grinder;
S3, the above-mentioned ball grinder that composite material is housed is vacuumized, be filled with inert gas;
S4, the ball grinder in step S3 is put on high energy ball mill and carried out ball milling, obtain disperse wild phase lightweight Mg-Ti solid solutionBody.
The average grain size of the pure magnesium dust of nanometer in above-mentioned steps S1 is 150-200nm, the pure titanium powder of nanometer flatAll crystallite dimension is 40-60nm.
In above-mentioned steps S1, the volume ratio of the pure magnesium dust of nanometer and the pure titanium powder of nanometer is 10:1-15:1.
The mass ratio of the composite material in above-mentioned steps S2 and stainless steel abrading-ball is 1:50-1:80.
In above-mentioned steps S2, the diameter of ball grinder is 20cm, and the quantity of the stainless steel abrading-ball in described spheroidal graphite tank is 2, instituteThe diameter of stating 2 stainless steel abrading-balls is respectively 10cm and 5cm. The stainless steel abrading-ball of different-diameter can make mixing in ball grinderClosing raw material is ground fully.
In above-mentioned steps S3, inert gas is more than 99% purity, and extracting vacuum number of times is 2-3 time, avoids in ball grinderThere is other gas, prevents under high temperature that the composite material in ball grinder produces in process of lapping oxidized.
Inert gas in above-mentioned steps S3 is preferably helium.
Drum's speed of rotation in above-mentioned steps S4 is 200-250 rev/min, and Ball-milling Time is 50-60h, every ball milling 30 minutes,Ball mill quits work 5 minutes.
The average grain size of the pure magnesium dust of above-mentioned nanometer is preferably 150nm, the average crystal grain of the pure titanium powder of described nanometerBe preferably dimensioned to be 40nm, the volume ratio of the pure magnesium dust of described nanometer and the pure titanium powder of nanometer is preferably 10:1, described composite materialBe preferably 1:50 with the mass ratio of stainless steel abrading-ball, described drum's speed of rotation is preferably 200h, and Ball-milling Time is preferably 50h.
Through in above-mentioned processing preparation process, utilize the energy that high energy ball mill provides can effectively overcome Mg-Ti admittedlySolution activation energy, the lattice that makes Ti atom enter into magnesium goes, and forms the Mg-Ti solid solution of disperse.
The present invention adopts the reason of Ti as disperse wild phase:
, compared with rare earth element and other alloying elements, Ti element all has the feature that specific strength is high, fusing point is high, andTi element is the same with Mg element, all has Patterns for Close-Packed Hexagonal Crystal structure, and it is good that the uniformity of this crystal structure has Ti and MgGood interface combination;
, Ti element compared with rare earth element, its relative density is lower, rare earth element is than great, and adopts rare earth element to doFor making magnesium and the light advantage of magnesium alloy materials quality, wild phase do not exist;
, simultaneously in the time of solid phase, Mg dissolves any Ti element in mutually hardly, and does not also find in existing documentThe existence of the intermetallic compound between Mg-Ti, this feature also makes Ti element can in magnesium and magnesium alloy materials, form surelyFixed disperse wild phase, is conducive to improve magnesium and magnesium alloy materials mechanical behavior under high temperature.
Usefulness of the present invention is: a kind of disperse wild phase lightweight Mg-Ti solid solution prepared that the present invention announcesMethod, preparation method is simple, and production cost is low, and finished product has excellent mechanical behavior under high temperature, has effectively solved routine castingMethod is difficult to produce the predicament of Mg-Ti solid solution, and Mg and the density of Ti element own are smaller, and Ti element is only 4.54g/cm3, shapeThe Mg-Ti solid solution becoming is given full play to the advantage that magnesium alloy materials quality is light; The Patterns for Close-Packed Hexagonal Crystal structure that Ti and Mg have,Make Ti and Mg have good combination interface, the lattice that Ti element enters into magnesium in the mode of disperse goes, and has effectively improvedThe properties of solid solution.
Brief description of the drawings
Fig. 1 is the preparation process of a kind of embodiment of the method 1 of preparing disperse wild phase lightweight Mg-Ti solid solution of the present inventionIn the XRD collection of illustrative plates of Mg-Ti solid solution.
Fig. 2 is that the Mg-Ti of a kind of embodiment of the method 1 of preparing disperse wild phase lightweight Mg-Ti solid solution of the present invention is solidThe lattice variations rule figure of solution.
Fig. 3 is that the Mg-Ti of a kind of embodiment of the method 1 of preparing disperse wild phase lightweight Mg-Ti solid solution of the present invention is solidThe Electronic Speculum figure of solution.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described. Following examples are only for more clearly illustrating the present inventionTechnical scheme, and can not limit the scope of the invention with this.
The pure magnesium dust of nanometer used in the present invention and the pure titanium powder of nanometer are that market is bought.
Embodiment 1:
A method of preparing disperse wild phase lightweight Mg-Ti solid solution, comprises the following steps: (1) by average grain size isThe pure magnesium dust of nanometer of 150nm and the pure titanium powder of nanometer that average grain size is 40nm are carried out proportioning with the volume ratio of 10:1;(2) above-mentioned composite material is sealed in the ball grinder that diameter is 20cm, wherein having 2 diameters in tank is 10cm and 20cmStainless steel abrading-ball, the mass ratio of composite material and stainless steel abrading-ball is 1:50; (3) the above-mentioned ball grinder that composite material is housed is taken out veryEmpty 3 times, being filled with purity is more than 99% helium protection; (4) ball grinder is put on planetary high-energy ball mill, ball mill turnsSpeed is 200 revs/min, and Ball-milling Time is 50h, every ball milling 30 minutes, and ball mill quits work 5 minutes, prevents temperature in ball grinderToo high.
Through in above-mentioned processing preparation process, utilize the energy that high energy ball mill provides can effectively overcome Mg-Ti admittedlySolution activation energy, the lattice that makes Ti atom enter into magnesium goes, and forms the Mg-Ti solid solution of disperse.
Embodiment 2:
A method of preparing disperse wild phase lightweight Mg-Ti solid solution, comprises the following steps: (1) by average grain size isThe pure magnesium dust of nanometer of 200nm and the pure titanium powder of nanometer that average grain size is 60nm are carried out proportioning with the volume ratio of 15:1;(2) above-mentioned composite material is sealed in the ball grinder that diameter is 20cm, wherein in tank, having diameter is two kinds of 10cm and 20cmDifferent stainless steel abrading-balls, the mass ratio of composite material and stainless steel abrading-ball is 1:80; (3) the above-mentioned ball milling that composite material is housedTank vacuumizes 2 times, and being filled with purity is more than 99% helium protection; (4) ball grinder is put on planetary high-energy ball mill to ballMill speed is 250 revs/min, and Ball-milling Time is 60h, every ball milling 30 minutes, and ball mill quits work 5 minutes, prevents ball grinderInterior excess Temperature.
Through in above-mentioned processing preparation process, utilize the energy that high energy ball mill provides can effectively overcome Mg-Ti admittedlySolution activation energy, the lattice that makes Ti atom enter into magnesium goes, and forms the Mg-Ti solid solution of disperse.
Embodiment 3:
A method of preparing disperse wild phase lightweight Mg-Ti solid solution, comprises the following steps: (1) by average grain size isThe pure magnesium dust of nanometer of 180nm and the pure titanium powder of nanometer that average grain size is 50nm are carried out proportioning with the volume ratio of 12:1;(2) above-mentioned composite material is sealed in the ball grinder that diameter is 20cm, wherein in tank, having diameter is two kinds of 10cm and 20cmDifferent stainless steel abrading-balls, the mass ratio of composite material and stainless steel abrading-ball is 1:60; (3) the above-mentioned ball milling that composite material is housedTank vacuumizes 3 times, and being filled with purity is more than 99% helium protection; (4) ball grinder is put on planetary high-energy ball mill to ballMill speed is 220 revs/min, and Ball-milling Time is 55h, every ball milling 30 minutes, and ball mill quits work 5 minutes, prevents ball grinderInterior excess Temperature.
Through in above-mentioned processing preparation process, utilize the energy that high energy ball mill provides can effectively overcome Mg-Ti admittedlySolution activation energy, the lattice that makes Ti atom enter into magnesium goes, and forms the Mg-Ti solid solution of disperse.
Embodiment 4:
A method of preparing disperse wild phase lightweight Mg-Ti solid solution, comprises the following steps: (1) by average grain size isThe pure magnesium dust of nanometer of 150nm and the pure titanium powder of nanometer that average grain size is 40nm are carried out proportioning with the volume ratio of 10:1;(2) above-mentioned composite material is sealed in the ball grinder that diameter is 20cm, wherein in tank, having diameter is two kinds of 10cm and 20cmDifferent stainless steel abrading-balls, the mass ratio of composite material and stainless steel abrading-ball is 1:80; (3) the above-mentioned ball milling that composite material is housedTank vacuumizes 2 times, and being filled with purity is more than 99% helium protection; (4) ball grinder is put on planetary high-energy ball mill to ballMill speed is 250 revs/min, and Ball-milling Time is 60h, every ball milling 30 minutes, and ball mill quits work 5 minutes, prevents ball grinderInterior excess Temperature. Through in above-mentioned processing preparation process, utilize the energy that high energy ball mill provides can effectively overcome Mg-TiSolid solution activation energy, the lattice that makes Ti atom enter into magnesium goes, and forms the Mg-Ti solid solution of disperse.
Embodiment 5:
A method of preparing disperse wild phase lightweight Mg-Ti solid solution, comprises the following steps: (1) just average grain sizeFor the pure titanium powder of nanometer that the pure magnesium dust of nanometer and the average grain size of 200nm are 60nm is carried out with the volume ratio (height) of 15:1Proportioning; (2) above-mentioned composite material is sealed in the ball grinder that diameter is 20cm, wherein in tank, having diameter is 10cm and 20cmTwo kinds of different stainless steel abrading-balls, the mass ratio of composite material and stainless steel abrading-ball is 1:50; (3) the above-mentioned composite material of being equipped withBall grinder vacuumizes 2 times, and being filled with purity is more than 99% helium protection; (4) ball grinder is put into planetary high-energy ball millUpper, drum's speed of rotation is 200 revs/min, and Ball-milling Time is 50h, every ball milling 30 minutes, and ball mill quits work 5 minutes, prevents ballExcess Temperature in grinding jar. Through in above-mentioned processing preparation process, utilize the energy that high energy ball mill provides effectively to overcomeMg-Ti solid solution activation energy, the lattice that makes Ti atom enter into magnesium goes, and forms the Mg-Ti solid solution of disperse.
Figure of description 1 is a kind of embodiment of the method 1 of preparing disperse wild phase lightweight Mg-Ti solid solution of the present inventionThe XRD collection of illustrative plates of the Mg-Ti solid solution in preparation process, as seen from the figure, along with the increase of Ball-milling Time, the diffraction of Mg and Ti in figurePeak intensity is more and more less, and in the time that Ball-milling Time is increased to 40h, in material, the diffraction peak intensity of Mg and Ti significantly declines, and Ti is describedAtom is attached in the lattice of magnesium and goes, and this stage, the Mg-Ti solid solution content in material increased rapidly along with the increase of Ball-milling TimeAdd Mg(Ti) content is corresponding falls sharply, until when ball milling 40h, Mg(Ti) diffraction maximum disappears, and formed Mg-Ti solid solution. After this,Continuing increases Ball-milling Time, and the thing phase composition of material substantially no longer changes.
Figure of description 2 is a kind of embodiment of the method 1 of preparing disperse wild phase lightweight Mg-Ti solid solution of the present inventionThe lattice variations rule figure of Mg-Ti solid solution, structure cell three length of side a, b of Mg-Ti solid solution crystals, c(lattice paprmeter) noEquate; In the time of a=b ≠ c, as seen from the figure, bottom surface lattice paprmeter a and the vertical lattice paprmeter c increase along with Ball-milling Time, numberValue diminishes gradually, and Ball-milling Time is to 50-60 hour, and lattice paprmeter variation tends towards stability, and the increase with Ball-milling Time is described, Mg-The lattice of Ti solid solution is more and more less, and when Ball-milling Time is to 50-60 hour, the variation of lattice tends towards stability.
Figure of description 3 is a kind of embodiment of the method 1 of preparing disperse wild phase lightweight Mg-Ti solid solution of the present inventionThe Electronic Speculum figure of Mg-Ti solid solution, as seen from the figure, the grain size of the Mg-Ti solid solution after ball milling is similar, and is evenly distributed, largeThe size of part crystal grain, in about 20-30nm, proves, it is nanometer material that the present invention adopts Mg-Ti solid solution prepared by ball-milling technologyMaterial.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for those skilled in the art, not departing under the prerequisite of the technology of the present invention principle, can also make some improvement and distortion, these improvement and distortion are alsoShould be considered as protection scope of the present invention.

Claims (9)

1. a method of preparing disperse wild phase lightweight Mg-Ti solid solution, comprises the following steps:
S1, pure nanometer magnesium dust and the pure titanium powder of nanometer are carried out to proportioning by volume make composite material;
S2, by above-mentioned composite material and stainless steel abrading-ball proportioning in mass ratio, be sealed in ball grinder;
S3, the above-mentioned ball grinder that composite material is housed is vacuumized, be filled with inert gas;
S4, the ball grinder in step S3 is put on high energy ball mill and carried out ball milling, obtain disperse wild phase lightweight Mg-Ti solid solutionBody.
2. a kind of method of preparing disperse wild phase lightweight Mg-Ti solid solution according to claim 1, is characterized in that,The average grain size of the pure magnesium dust of nanometer in described step S1 is 150-200nm, the average crystal grain chi of the pure titanium powder of nanometerVery little is 40-60nm.
3. a kind of method of preparing disperse wild phase lightweight Mg-Ti solid solution according to claim 1, is characterized in that,In described step S1, the volume ratio of the pure magnesium dust of nanometer and the pure titanium powder of nanometer is 10:1-15:1.
4. a kind of method of preparing disperse wild phase lightweight Mg-Ti solid solution according to claim 1, is characterized in that,The mass ratio of the composite material in described step S2 and stainless steel abrading-ball is 1:50-1:80.
5. a kind of method of preparing disperse wild phase lightweight Mg-Ti solid solution according to claim 1, is characterized in that,In described step S2, the diameter of ball grinder is 20cm, and the quantity of the stainless steel abrading-ball in described spheroidal graphite tank is 2, described 2 notThe diameter of rust steel abrading-ball is respectively 10cm and 5cm.
6. a kind of method of preparing disperse wild phase lightweight Mg-Ti solid solution according to claim 1, is characterized in that,Inert gas in described step S3 is more than 99% purity.
7. a kind of method of preparing disperse wild phase lightweight Mg-Ti solid solution according to claim 1, is characterized in that,Inert gas in described step S3 is helium.
8. a kind of method of preparing disperse wild phase lightweight Mg-Ti solid solution according to claim 1, is characterized in that instituteThe drum's speed of rotation of stating in step S4 is 200-250 rev/min, and Ball-milling Time is 50-60h, every ball milling 30 minutes, and ball mill stopsWork 5 minutes.
9. a kind of method of preparing disperse wild phase lightweight Mg-Ti solid solution according to claim 1, is characterized in that,The average grain size of the pure magnesium dust of described nanometer is 150nm, and the average grain size of the pure titanium powder of described nanometer is 40nm, instituteThe volume ratio of stating the pure magnesium dust of nanometer and the pure titanium powder of nanometer is 10:1, and the mass ratio of described composite material and stainless steel abrading-ball is1:50, described drum's speed of rotation is 200h, Ball-milling Time is 50h.
CN201610162567.8A 2016-03-22 2016-03-22 Method for preparing dispersed reinforced phase light Mg-Ti solid solution Pending CN105603230A (en)

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CN107243639A (en) * 2017-05-11 2017-10-13 广西大学 A kind of preparation method of supersaturated Mg (Ti) metal solid solution powder
CN107385252A (en) * 2017-08-03 2017-11-24 哈尔滨工业大学 A kind of preparation method of Ti dispersion-strengthernings Ultra-fine Grained high-strength magnesium alloy
CN109689907A (en) * 2016-09-07 2019-04-26 麻省理工学院 Containing titanium alloy and relevant manufacturing method
CN110976888A (en) * 2019-12-24 2020-04-10 郑州大学 Complete solid solution molybdenum-niobium alloy powder and preparation method and application thereof
US11634797B2 (en) 2013-03-14 2023-04-25 Massachusetts Institute Of Technology Sintered nanocrystalline alloys
US11644288B2 (en) 2015-09-17 2023-05-09 Massachusetts Institute Of Technology Nanocrystalline alloy penetrators

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CN103551583A (en) * 2013-11-21 2014-02-05 哈尔滨工业大学 Preparation method for Mg-Ti alloy powder
CN105170972A (en) * 2015-09-02 2015-12-23 中南大学 Mg-Ti hydrogen storage alloy powder and preparation method thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11634797B2 (en) 2013-03-14 2023-04-25 Massachusetts Institute Of Technology Sintered nanocrystalline alloys
US11674205B2 (en) 2013-03-14 2023-06-13 Massachusetts Institute Of Technology Alloys comprising chromium and second metal material
US11644288B2 (en) 2015-09-17 2023-05-09 Massachusetts Institute Of Technology Nanocrystalline alloy penetrators
CN109689907A (en) * 2016-09-07 2019-04-26 麻省理工学院 Containing titanium alloy and relevant manufacturing method
CN107243639A (en) * 2017-05-11 2017-10-13 广西大学 A kind of preparation method of supersaturated Mg (Ti) metal solid solution powder
CN107385252A (en) * 2017-08-03 2017-11-24 哈尔滨工业大学 A kind of preparation method of Ti dispersion-strengthernings Ultra-fine Grained high-strength magnesium alloy
CN110976888A (en) * 2019-12-24 2020-04-10 郑州大学 Complete solid solution molybdenum-niobium alloy powder and preparation method and application thereof

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