CN104805318A - Preparation method of spherical TC4 particle reinforced AZ91 magnesium matrix composite - Google Patents

Preparation method of spherical TC4 particle reinforced AZ91 magnesium matrix composite Download PDF

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CN104805318A
CN104805318A CN201510178251.3A CN201510178251A CN104805318A CN 104805318 A CN104805318 A CN 104805318A CN 201510178251 A CN201510178251 A CN 201510178251A CN 104805318 A CN104805318 A CN 104805318A
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spherical
matrix composite
preparation
magnesium matrix
particulate reinforced
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CN104805318B (en
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王晓军
张春雷
胡小石
吴昆�
郑明毅
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention relates to a preparation method of a reinforced AZ91 magnesium matrix composite, in particular to a preparation method of a spherical TC4 particle reinforced AZ91 magnesium matrix composite, and aims to provide a new method for preparing the TC4/magnesium matrix composite. The method comprises steps as follows: 1, preheating of TC4 particles; 2, semi-solid state stirring; 3, ultrasonic treatment; 4, self-settlement; 5, cooling. Therefore, the spherical TC4 particle reinforced AZ91 magnesium matrix composite is prepared.

Description

A kind of preparation method of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite
Technical field
The present invention relates to the control that spherical TC4 particle and AZ91 basal body interface react, make there is good interface cohesion between the two, thus obtain the matrix material of good over-all properties.
Background technology
Generally adopt ceramic particle as the reinforcement of magnesium base composite material at present, as SiC, B 4c, TiC, TiC, Al 2o 3, Y 2o 3, TiO 2, Mg 2si etc., but due to the bad performance of material that causes of wettability between ceramic phase and matrix such as SiC bad.And wettability between titanium and magnesium is good especially, and physicochemical property are similar, and therefore the present invention adopts Ti particle as the reinforcement of matrix material, are expected to obtain the magnesium base composite material that intensity is high and plasticity and toughness are good.
Summary of the invention
The object of the invention is to provide a kind of novel method of the TC4/ of preparation magnesium base composite material: TC4 particle is joined in AZ91 melt, make particle sedimentation under gravity, the time of control settlement, by water-cooling system, melt is cooled fast subsequently, thus obtain high-volume fractional and the magnesium base composite material of particle distribution gradient.
The method of the present invention from sedimentation makes particle sedimentation under gravity, and water-cooled is solidified rapidly subsequently, thus obtains the as cast condition matrix material of particle distribution gradient, enables material be more applicable for the demand of people.
The preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite of the present invention, it comprises the following steps:
One, TC4 particle preheating: by TC4 particle preheating 30 ~ 60min at 50 ~ 100 DEG C;
Two, Semi-solid Stirring: first AZ91 is heated to 560 ~ 620 DEG C, make AZ91 be melted to semi-solid state, then join in AZ91 semi-solid melt by the TC4 particle of step one preheating with the speed of 120g/min, limit edged stirs, continue stirring 20 ~ 30min again after adding, obtain mixture;
Three, supersound process: mixture step 2 obtained carries out supersound process, ultrasonic frequency is 20kHz, and ultrasonic time is 20 ~ 30min;
Four, from sedimentation: the mixture after step 3 supersound process is left standstill 20 ~ 30min naturally, makes spherical TC4 particles settling;
Five, cool: by the melt cooling of settlement treatment in step 4, obtain the matrix material of as cast condition, namely complete described spherical TC4 particulate reinforced AZ 91 magnesium matrix composite.
The present invention comprises following advantage:
The present invention adopts and strengthens magnesium base composite material from sedimentation legal system for titanium alloy particle, first being heated up by magnesium alloy lowers the temperature afterwards forms semi-solid state, then titanium alloy particle preheated is in advance poured in semi-solid melt and carries out Semi-solid Stirring simultaneously, after stirring the scheduled time, blend melt is warming up to liquid state, carry out ultrasonication subsequently, and melt is cooled in water-cooling system obtain as cast condition matrix material.
(1) the present invention will carry out heating, drying to titanium alloy particle in preparation process, and preheating temperature is 100 DEG C ~ 200 DEG C, warm up time is 20min ~ 50min, so both can reduce the gas volume being adsorbed on particle surface, improve the wettability between particle and alloy substrate, be conducive to the dispersion of particle, be unlikely to that again titanium alloy particle is oxidized serious, if preheating temperature is too high, particle surface will be made to form fine and close TiO 2layer, this ceramic phase is just spaced the combination between titanium alloy particle and matrix, and interface cohesion between particle and matrix can be caused poor;
(2) the present invention adopts liquid method to prepare matrix material, this is because the wettability of titanium particle and magnesium matrix is fine, compared to the method with powder metallurgy, the interface cohesion between the composite material granular that this method arrives and matrix is better.
(3) the present invention by making particle sedimentation under gravity from the method for sedimentation, and can obtain the gradient composites of particle distribution gradient in the height direction.
(4) the present invention can prepare the matrix material of higher volume fraction.
Accompanying drawing explanation
Fig. 1 is optical microscope photograph (OM) photo of the TC4 particulate reinforced AZ 91 magnesium matrix composite that the present invention obtains;
Fig. 2 is photo (SEM) photo of the scanning electronic microscope of TC4 particulate reinforced AZ 91 magnesium matrix composite prepared by the present invention;
Fig. 3 is Fracture scan (SEM) photo of the tension specimen of TC4 particulate reinforced AZ 91 magnesium matrix composite prepared by the present invention;
Fig. 4 is the compression test curve of the TC4 particulate reinforced AZ 91 magnesium matrix composite prepared of the present invention and AZ91 alloy.
Embodiment
Embodiment one: the preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite of present embodiment, it comprises the following steps:
One, TC4 particle preheating: by TC4 particle preheating 30 ~ 60min at 50 ~ 100 DEG C;
Two, Semi-solid Stirring: first AZ91 is heated to 560 ~ 620 DEG C, make AZ91 be melted to semi-solid state, then join in AZ91 semi-solid melt by the TC4 particle of step one preheating with the speed of 120g/min, limit edged stirs, continue stirring 20 ~ 30min again after adding, obtain mixture;
Three, supersound process: mixture step 2 obtained carries out supersound process, ultrasonic frequency is 20kHz, and ultrasonic time is 20 ~ 30min;
Four, from sedimentation: the mixture after step 3 supersound process is left standstill 20 ~ 30min naturally, makes spherical TC4 particles settling;
Five, cool: by the melt cooling of settlement treatment in step 4, obtain the matrix material of as cast condition, namely complete described spherical TC4 particulate reinforced AZ 91 magnesium matrix composite.
Embodiment two: present embodiment and embodiment one unlike: the particle preheating temperature described in step one is 60 DEG C ~ 100 DEG C.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one unlike: the particle preheating temperature described in step one is 70 DEG C ~ 100 DEG C.Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one unlike: the particle preheating temperature described in step one is 80 DEG C ~ 100 DEG C.Other is identical with embodiment one.
Embodiment five: present embodiment and embodiment one unlike: the particle preheating temperature described in step one is 90 DEG C ~ 100 DEG C.Other is identical with embodiment one.
Embodiment six: present embodiment and embodiment one unlike: in step 2, AZ91 is heated to 570 ~ 610 DEG C.Other is identical with embodiment one.
Embodiment seven: present embodiment and embodiment one unlike: in step 2, AZ91 is heated to 580 ~ 600 DEG C.Other is identical with embodiment one.
Embodiment eight: present embodiment and embodiment one unlike: in step 2, AZ91 is heated to 590 ~ 600 DEG C.Other is identical with embodiment one.
Embodiment nine: present embodiment and embodiment one unlike: the cross stirring rake of the whipping process described in step 2, stirring velocity is 1000r/min.Other is identical with embodiment one.
Embodiment ten: present embodiment and embodiment one unlike: before mixture carries out supersound process in step 3, first the mixture in step 2 is warmed up to 690 DEG C, and then carries out ultrasonication.Other is identical with embodiment one.
Embodiment 11: present embodiment and embodiment one unlike: the ultrasonic frequency of the supersound process described in step 3 is 20kHz, and ultrasonic time is 20min.Other is identical with embodiment one.
Embodiment 12: present embodiment and embodiment one unlike: the temperature from settling process described in step 4 is 690 DEG C, and the settling time is 20min.Other is identical with embodiment one.
Embodiment 13: present embodiment and embodiment one unlike: what mixture process of cooling utilized in step 5 is that circulating water cooling system carries out.Other is identical with embodiment one.
Following examples are provided below in conjunction with content of the present invention:
Embodiment 1:
Getting 624g diameter is that the TC4 spheroidal particle of 109 μm-150 μm is put in the cup of a porcelain, puts in the resistance heading furnace of cup and 100 DEG C and keeps 30min;
Quality be meanwhile 1000g AZ91 alloy 720 DEG C fusing and progressively cool to 580 DEG C (semi-solid states); Subsequently stirring rake is reached appropriate location under melt liquid level, start stirring rake, preheated particle is taken out and slowly joins in melt, this process will adjust rotating speed enables particle enter into melt smoothly, at the uniform velocity (1000r/min) is stirred after particle adds, stir 20min, then temperature is elevated to 690 DEG C, stop stirring; Unload lower stirring paddle subsequently, start supersound process, default ultrasonic frequency is 20kHz, and output rating is 700W, and this process carries out 20min; Subsequently melt is left standstill 20min in gravity field, finally rapid being put in water-cooling system by the crucible taking up melt cools, and what this water-cooling system utilized is circulating water, only needs the TC4 particulate reinforced AZ 91 magnesium matrix composite that can obtain as cast condition for a minute.Matrix material is placed on scanning electron microscope and optical fiber Microscopic observation.
Optical microscope photograph (OM) photo of the TC4 particulate reinforced AZ 91 magnesium matrix composite that the present embodiment obtains as shown in Figure 1; Photo (SEM) photo of the scanning electronic microscope of TC4 particulate reinforced AZ 91 magnesium matrix composite as shown in Figure 2; Fracture scan (SEM) photo of the tension specimen of TC4 particulate reinforced AZ 91 magnesium matrix composite as shown in Figure 2; The compression test curve of TC4 particulate reinforced AZ 91 magnesium matrix composite and AZ91 alloy as shown in Figure 4.
From the above, the method for the present embodiment can prepare the matrix material of higher volume fraction.

Claims (10)

1. a preparation method for spherical TC4 particulate reinforced AZ 91 magnesium matrix composite, is characterized in that it comprises the following steps:
One, TC4 particle preheating: by TC4 particle preheating 30 ~ 60min at 50 ~ 100 DEG C;
Two, Semi-solid Stirring: first AZ91 is heated to 560 ~ 620 DEG C, make AZ91 be melted to semi-solid state, then join in AZ91 semi-solid melt by the TC4 particle of step one preheating with the speed of 120g/min, limit edged stirs, continue stirring 20 ~ 30min again after adding, obtain mixture;
Three, supersound process: mixture step 2 obtained carries out supersound process, ultrasonic frequency is 20kHz, and ultrasonic time is 20 ~ 30min;
Four, from sedimentation: the mixture after step 3 supersound process is left standstill 20 ~ 30min naturally, makes spherical TC4 particles settling;
Five, cool: by the melt cooling of settlement treatment in step 4, obtain the matrix material of as cast condition, namely complete described spherical TC4 particulate reinforced AZ 91 magnesium matrix composite.
2. the preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite according to claim 1, is characterized in that the particle preheating temperature described in step one is 70 DEG C ~ 100 DEG C.
3. the preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite according to claim 2, is characterized in that the particle preheating temperature described in step one is 80 DEG C ~ 100 DEG C.
4. the preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite according to claim 1, is characterized in that, in step 2, AZ91 is heated to 570 ~ 600 DEG C.
5. the preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite according to claim 4, is characterized in that, in step 2, AZ91 is heated to 580 ~ 600 DEG C.
6. the preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite according to claim 1, it is characterized in that the cross stirring rake of the whipping process described in step 2, stirring velocity is 1000r/min.
7. the preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite according to claim 1, before it is characterized in that in step 3, mixture carries out supersound process, first the mixture in step 2 is warmed up to 690 DEG C, and then carries out ultrasonication.
8. the preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite according to claim 1, it is characterized in that the ultrasonic frequency of the supersound process described in step 3 is 20kHz, ultrasonic time is 20min.
9. the preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite according to claim 1, it is characterized in that the temperature from settling process described in step 4 is 690 DEG C, the settling time is 20min.
10. the preparation method of a kind of spherical TC4 particulate reinforced AZ 91 magnesium matrix composite according to claim 1, it is characterized in that in step 5 by mixture process of cooling utilize be that circulating water cooling system carries out.
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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN108179412A (en) * 2018-01-25 2018-06-19 成都青石激光科技有限公司 The method for preparing spheric granules composite material
CN108677053A (en) * 2018-06-22 2018-10-19 太原理工大学 A kind of preparation method for handing over frequency ultrasonic coupling hot pressing infiltration porous ceramics enhancing magnesium-based composite material
CN109022859A (en) * 2018-09-17 2018-12-18 太原理工大学 A kind of preparation method of nano-titanium particulate reinforcement magnesium-based composite material
CN112342445A (en) * 2020-09-10 2021-02-09 上海航天精密机械研究所 High-strength plastic magnesium-based composite material and preparation method thereof
CN113046592A (en) * 2021-03-16 2021-06-29 南昌航空大学 In-situ synthesis device and method for aluminum-based composite material with enhanced particle gradient distribution
CN113373359A (en) * 2021-06-23 2021-09-10 贵州大学 Layered gradient structure particle reinforced magnesium matrix composite material and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108179412A (en) * 2018-01-25 2018-06-19 成都青石激光科技有限公司 The method for preparing spheric granules composite material
CN108677053A (en) * 2018-06-22 2018-10-19 太原理工大学 A kind of preparation method for handing over frequency ultrasonic coupling hot pressing infiltration porous ceramics enhancing magnesium-based composite material
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CN112342445A (en) * 2020-09-10 2021-02-09 上海航天精密机械研究所 High-strength plastic magnesium-based composite material and preparation method thereof
CN113046592A (en) * 2021-03-16 2021-06-29 南昌航空大学 In-situ synthesis device and method for aluminum-based composite material with enhanced particle gradient distribution
CN113373359A (en) * 2021-06-23 2021-09-10 贵州大学 Layered gradient structure particle reinforced magnesium matrix composite material and preparation method thereof

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