CN109402540A - A method of eliminating particle enhances AZ91D magnesium-based composite material dislocation - Google Patents

A method of eliminating particle enhances AZ91D magnesium-based composite material dislocation Download PDF

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Publication number
CN109402540A
CN109402540A CN201811514097.2A CN201811514097A CN109402540A CN 109402540 A CN109402540 A CN 109402540A CN 201811514097 A CN201811514097 A CN 201811514097A CN 109402540 A CN109402540 A CN 109402540A
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CN
China
Prior art keywords
composite material
based composite
stirring
rolling
az91d magnesium
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CN201811514097.2A
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Chinese (zh)
Inventor
李惠
焦雷
王兴波
徐品
徐品一
陆圣波
孔德福
邹洋
于淼
李明峰
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Jiangsu University of Science and Technology
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Jiangsu University of Science and Technology
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Priority to CN201811514097.2A priority Critical patent/CN109402540A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon

Abstract

The invention discloses a kind of methods of elimination particle enhancing AZ91D magnesium-based composite material dislocation, belong to magnesium-based composite material technical field of modification.It is characterized by: passing through conjunctive use rolling and agitating friction Combined machining, the size shape of particle enhancing AZ91D magnesium-based composite material reinforcement is set to change and redistribute, AZ91D magnesium-based composite material matrix grain recrystallizes, distortion of lattice is reduced, it realizes the purpose for eliminating particle enhancing AZ91D magnesium-based composite material dislocation, and further increases the comprehensive performance of AZ91D magnesium-based composite material.

Description

A method of eliminating particle enhances AZ91D magnesium-based composite material dislocation
Technical field
The present invention relates to AZ91D magnesium-based composite materials, belong to technical field of material modification, and in particular to a kind of elimination particle increasing The method of strong AZ91D magnesium-based composite material dislocation.
Background technique
AZ91D magnesium-based composite material specific strength with higher, specific stiffness, while also there is preferable wearability, resistance to height Warm, lower thermal expansion coefficient and damping performance.In addition, AZ91D magnesium-based composite material also has good damping capacity and electricity Magnetic shield performance is good functional material.Particle enhances low AZ91D magnesium-based composite material preparation cost, simple process and tool Standby isotropism is the AZ91D magnesium-based composite material of most possible realization low-coat scale commodity production at present.Therefore, Grain enhancing AZ91D magnesium-based composite material has sizable application prospect in the industry such as electronics, aerospace, automobile.But Due to the presence of dislocation, causes material that distortion of lattice occurs, cause toughness of material low, brittleness is big, and processing performance is low.Research hair Existing, microstructure modification technology can eliminate particle enhancing AZ91D magnesium-based composite material dislocation, and improving particle enhances AZ91D magnesium-based The comprehensive performance of composite material.Therefore, the material modification method for eliminating particle enhancing AZ91D magnesium-based composite material dislocation is ground Study carefully personnel's concern.
It is retrieved through applicant, the research about AZ91D magnesium-based composite material dislocation is mainly around dislocation motion, dislocation at present Proliferation, dislocation strengthening etc., Hong Chengmiao have studied the movement of particle enhancing AZ91D magnesium-based composite material dislocation, proliferation, Nan Hong Proliferation, the entanglement etc. for having studied particle enhancing AZ91D magnesium-based composite material dislocation by force, do not find so far by eliminating particle Enhancing AZ91D magnesium-based composite material dislocation improves the patent of its comprehensive performance.
Summary of the invention
Goal of the invention: to overcome the shortcomings of the above technology, it is an object of that present invention to provide improve particle to enhance AZ91D magnesium-based The technical method of composite material combination property is especially to provide a kind of elimination particle enhancing AZ91D magnesium-based composite material dislocation Method.
Technical solution: to realize that above-mentioned technical characteristic, elimination particle proposed by the present invention enhance AZ91D magnesium-based composite material The method of dislocation the following steps are included:
(1) block particle enhancing AZ91D magnesium-based composite material ingot casting is subjected to rolling process, be prepared into certain thickness AZ91D magnesium-based composite material plate;
(2) the particle enhancing AZ91D magnesium-based composite material after rolling is stirred friction working process.
After completion of processing, TEM microexamination and XRD characterization test are carried out, the results showed that number of dislocations is a large amount of with density It reduces and even disappears, it is wear-resisting to be improved with comprehensive performances such as intensity.
Wherein, the enhancing grain volume fraction of the particle enhancing AZ91D magnesium-based composite material is 5vol.%- 10vol.%.If enhancing grain volume fraction it is excessively high, material too stiff plastic is poor, cause stirring-head can fracture failure, and The too low material of grain content is too soft, and material can be stirred head and blend.
Preferably, the technological parameter of rolling process are as follows: 420-450 DEG C of rolling temperature;Rolling thickness is to 4-6mm.
It is highly preferred that in rolling, by multi- pass rolling, volume under pressure 0.5-0.6mm per pass.
Preferably, mixing yoghurt processing is carried out after rolling, mixing yoghurt technological parameter position: stirring-head revolving speed: 1200-1500r/min;Stirring-head process velocity: 80-120mm/min;The shoulder breadth diameter of stirring-head: 10~15mm;Stir scalp acupuncture It is long: 3~3.5mm;Mixing needle diameter: 3~5mm;Test volume under pressure are as follows: 2~2.5mm;Stirring-head with it is vertical aspect inclination angle be 3.0~5.0 degree;The stirring of single side multi-pass;Overlapping rate 20~30%.
It is highly preferred that the shoulder breadth diameter of stirring-head: 15mm;It is long to stir scalp acupuncture: 3.5mm;Mixing needle diameter: 5mm;Under test Pressure amount are as follows: 2.5mm;Stirring-head is 3.0 degree with the inclination angle of vertical aspect;The stirring of single side multi-pass;Overlapping rate 30%.
Present invention focuses on rolling to stir to combine dislocation, single roll cannot achieve dislocation with single stirring.Particularly, lead to The repeat region and control overlapping rate for crossing control stirring, achieve the purpose that eliminate dislocation.
In one preferred embodiment, technical solution of the present invention is achieved by the steps of:
(1) block particle enhancing AZ91D magnesium-based composite material ingot casting is rolled, is prepared into certain thickness AZ91D Magnesium-based composite material plate;Rolling process technological parameter: 420-450 DEG C of rolling temperature;Rolling thickness is to 4-6mm;By multi-pass It rolls, per pass volume under pressure 0.5-0.6mm.
(2) the particle enhancing AZ91D magnesium-based composite material after rolling is stirred friction working process;Agitating friction adds Work technological parameter: stirring-head revolving speed: 1200-1500r/min;Stirring-head process velocity: 80-120mm/min;The shoulder breadth of stirring-head Diameter: 15mm;It is long to stir scalp acupuncture: 3.5mm;Mixing needle diameter: 5mm;Test volume under pressure are as follows: 2.5mm;Stirring-head with it is vertical aspect Inclination angle be 3.0 degree;The stirring of single side multi-pass;Overlapping rate 30%.
(3) completion of processing, carries out TEM microexamination and XRD characterization test, and number of dislocations largely reduces or even disappears with density It loses, it is wear-resisting to be improved with comprehensive performances such as intensity.
It is compound largely to eliminate AZ91D magnesium-based by the way that rolling and mixing yoghurt technique is used in combination for the method for the present invention The dislocation of material, through TEM and the XRD characterization testing inspection analysis dislocation density ρ order of magnitude by 1014Drop to 103, number of dislocations is big Width decline, furthermore this method refines AZ91D magnesium-based composite material matrix crystal grain, improves the microstructure of enhancing particle, compared with The comprehensive performance of particle enhancing AZ91D magnesium-based composite material is improved well.The characteristics of the method for the present invention, is: after processing AZ91D magnesium-based composite material dislocation substantially eliminates, and carries out tensile test at room temperature, tensile strength, elongation percentage etc. significantly improve. Present device is simple and convenient to operate, success rate is high, low in cost, practical, is a kind of novel, efficient, practical particle Enhance AZ91D magnesium-based composite material dislocation and eliminates technique.
Specific embodiment
Embodiment 1:
The outer adding type volume fraction of working process is 8vol.%SiC/AZ91 composite material, specific implementation method:
(1) outer adding type 8vol.%SiC/AZ91 composite material slab 1000g is taken, 4mm thickness is rolled to using hot rolling process Degree, 420 DEG C of rolling temperature, by multi- pass rolling, volume under pressure 0.5mm per pass.
(2) material after rolling is cut into having a size of 200mm × 50mm × 4mm, in order to clamping, agitating friction rotary needle Go deep into general 3.5mm of Workpiece length or so;
(3) specimen clamping is fixed, is stirred friction working process, technological parameter is: stirring-head revolving speed: 1200r/ min;Stirring-head process velocity: 100mm/min;The shoulder breadth diameter of stirring-head: 15mm;It is long to stir scalp acupuncture: 3.5mm;Mixing needle is straight Diameter: 5mm;Test volume under pressure are as follows: 2.5mm;Stirring-head is 3.0 degree with the inclination angle of vertical aspect;The stirring of single side multi-pass;Overlapping rate 30%.
(4) after stirring friction treatment, with the dislocation of tem observation and XRD characterization experimental observation material internal, through TEM and XRD The testing inspection analysis dislocation density ρ order of magnitude is characterized by 1014Drop to 103, residual stress declines to a great extent, and carries out room temperature tensile It is tested with hardness test.The experimental results showed that even disappearance is greatly decreased in composite inner dislocation after the method for the present invention, Tensile strength has been increased to 4.2%, elongation percentage and has been increased to 15.2%, and hardness reduces 0.5%.
Embodiment 2:
Working process original position volume fraction is 6vol.%ZrB2/ AZ91 composite material, specific implementation method:
(1) 5vol.%ZrB in situ is taken2/ AZ61 composite material slab 1000g, is rolled to 5mm thickness using hot rolling process, 440 DEG C of rolling temperature, by multi- pass rolling, volume under pressure 0.6mm per pass.
(2) material after rolling is cut into having a size of 150mm × 50mm × 5mm;
(3) specimen clamping is fixed, is stirred friction working process, technological parameter is: stirring-head revolving speed: 1400r/ min;Stirring-head process velocity: 80mm/min;The shoulder breadth diameter of stirring-head: 15mm;It is long to stir scalp acupuncture: 3.5mm;Mixing needle is straight Diameter: 5mm;Test volume under pressure are as follows: 2.5mm;Stirring-head is 3.0 degree with the inclination angle of vertical aspect;The stirring of single side multi-pass;Overlapping rate 30%.
(4) after agitating friction, with the dislocation of tem observation and XRD characterization experimental observation material internal, through TEM and XRD characterization Testing inspection analyzes the dislocation density ρ order of magnitude by 1015Drop to 102, and carry out room temperature tensile and hardness test experiment.As a result table Bright, composite inner dislocation, which is reduced, after the method for the present invention even disappears, and tensile strength has been increased to 5.1%, elongation percentage It is increased to 16.3%, hardness reduces 0.3%.
Embodiment 3:
Working process original position volume fraction be 10vol.%AlN/AZ91 composite material, specific implementation method:
(1) 10vol.%AlN/AZ63 composite material slab 1000g in situ is taken, 6mm thickness is rolled to using hot rolling process, 450 DEG C of rolling temperature, by multi- pass rolling, volume under pressure 0.5mm per pass.
(2) material after rolling is cut into having a size of 150mm × 50mm × 6mm
(3) specimen clamping is fixed, is stirred friction working process, technological parameter is: stirring-head revolving speed: 1200r/ min;Stirring-head process velocity: 80mm/min;The shoulder breadth diameter of stirring-head: 15mm;It is long to stir scalp acupuncture: 3.5mm;Mixing needle is straight Diameter: 5mm;Test volume under pressure are as follows: 2.5mm;Stirring-head is 3.0 degree with the inclination angle of vertical aspect;The stirring of single side multi-pass;Overlapping rate 30%.
(4) after stirring friction treatment, with the dislocation of tem observation and XRD characterization experimental observation material internal, through TEM and XRD The testing inspection analysis dislocation density ρ order of magnitude is characterized by 1014Drop to 102, residual stress declines to a great extent, and carries out room temperature tensile It is tested with hardness test.The experimental results showed that even disappearance is greatly decreased in composite inner dislocation after the method for the present invention, Tensile strength has been increased to 5.9%, elongation percentage and has been increased to 17.1%, and hardness reduces 0.4%.
In conclusion the method for the present invention passes through conjunctive use rolling and mixing yoghurt technology (Friction Stir Processing, abbreviation FSP) it is combined processing, material is rolled first, the microstructure of material changes, and obtains To a large amount of texture, it is then stirred friction treatment, generates frictional heat using high-speed rotating stirring-head and material interaction Make material softening, the rotation and traveling of stirring-head make material part region dynamic recovery and recrystallization, lead to the microcosmic of material Institutional framework changes again.It is handled by two different material modification technical tie-ups, material matrix and enhancing body tissue Shape size changes, and is distributed dense uniform, and distortion of lattice is reduced, and dislocation is eliminated.The technology of the present invention is mainly characterized by using rolling System and the united combination process of mixing yoghurt, to more thoroughly eliminate the position of particle enhancing AZ91D magnesium-based composite material Mistake improves its comprehensive performance.Present invention process is simple and convenient to operate, success rate is high, low in cost, practical, is a kind of new Type, efficient, practical AZ91D magnesium-based composite material dislocation eliminate technique.

Claims (6)

1. it is a kind of eliminate particle enhancing AZ91D magnesium-based composite material dislocation method, characterization method the following steps are included:
(1) block particle enhancing AZ91D magnesium-based composite material ingot casting is subjected to rolling process, is prepared into certain thickness AZ91D Magnesium-based composite material plate;
(2) the particle enhancing AZ91D magnesium-based composite material after rolling is stirred friction working process.
2. the method according to claim 1, wherein the enhancing of particle enhancing AZ91D magnesium-based composite material Grain volume fraction is 5vol.%-10vol.%.
3. the method according to claim 1, wherein the technological parameter of rolling process are as follows: rolling temperature 420-450 ℃;Rolling thickness is to 4-6mm.
4. according to the method described in claim 3, it is characterized in that, in rolling, by multi- pass rolling, volume under pressure per pass 0.5-0.6mm。
5. the method according to claim 1, wherein carrying out mixing yoghurt processing, agitating friction after rolling Working process parameter position: stirring-head revolving speed: 1200-1500r/min;Stirring-head process velocity: 80-120mm/min;Stirring-head Shoulder breadth diameter: 10~15mm;It is long to stir scalp acupuncture: 3~3.5mm;Mixing needle diameter: 3~5mm;Test volume under pressure are as follows: 2~ 2.5mm;Stirring-head is 3.0~5.0 degree with the inclination angle of vertical aspect;The stirring of single side multi-pass;Overlapping rate 20~30%.
6. according to the method described in claim 5, it is characterized in that, the shoulder breadth diameter of stirring-head: 15mm;It is long to stir scalp acupuncture: 3.5mm;Mixing needle diameter: 5mm;Test volume under pressure are as follows: 2.5mm;Stirring-head is 3.0 degree with the inclination angle of vertical aspect;Single side is more Passage stirring;Overlapping rate 30%.
CN201811514097.2A 2018-12-11 2018-12-11 A method of eliminating particle enhances AZ91D magnesium-based composite material dislocation Pending CN109402540A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002205177A (en) * 2000-12-28 2002-07-23 Showa Denko Kk Friction stir welding method
CN101760710A (en) * 2008-12-24 2010-06-30 中国科学院金属研究所 Preparation method of fine crystalline superplastic heat-resistance magnesium alloy
CN102528271A (en) * 2012-01-20 2012-07-04 重庆大学 Method for improving mechanical property of FSW (friction stir welding) magnesium alloy joint
JP2012143811A (en) * 2010-12-24 2012-08-02 Sumitomo Electric Ind Ltd Magnesium alloy material
CN103668013A (en) * 2013-11-12 2014-03-26 江苏大学 Method for super-plastic pretreatment of in situ aluminum base composite material
JP2015057292A (en) * 2013-08-09 2015-03-26 国立大学法人大阪大学 Friction agitation joint method of metal
CN105463353A (en) * 2015-11-23 2016-04-06 哈尔滨工业大学 Method for manufacturing fine-grain magnesium alloy block through friction stir treatment
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Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002205177A (en) * 2000-12-28 2002-07-23 Showa Denko Kk Friction stir welding method
CN101760710A (en) * 2008-12-24 2010-06-30 中国科学院金属研究所 Preparation method of fine crystalline superplastic heat-resistance magnesium alloy
JP2012143811A (en) * 2010-12-24 2012-08-02 Sumitomo Electric Ind Ltd Magnesium alloy material
CN102528271A (en) * 2012-01-20 2012-07-04 重庆大学 Method for improving mechanical property of FSW (friction stir welding) magnesium alloy joint
JP2015057292A (en) * 2013-08-09 2015-03-26 国立大学法人大阪大学 Friction agitation joint method of metal
CN103668013A (en) * 2013-11-12 2014-03-26 江苏大学 Method for super-plastic pretreatment of in situ aluminum base composite material
CN105463353A (en) * 2015-11-23 2016-04-06 哈尔滨工业大学 Method for manufacturing fine-grain magnesium alloy block through friction stir treatment
CN106736269A (en) * 2016-12-01 2017-05-31 中国科学院金属研究所 A kind of preparation method of circular aluminum matrix composite silk material

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Title
B.N. SAHOOA ET AL.: "Microstructural modification and its effect on strengthening mechanism and yield asymmetry of in-situ TiC-TiB2/ AZ91 magnesium matrix", 《MATERIALS SCIENCE & ENGINEERING A》 *
柴方: "水下搅拌摩擦加工AZ系镁合金组织演变和变形机理的研究", 《中国博士学位论文全文数据库(电子期刊)工程科技I辑》 *

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