CN102899517A - In-situ SiC-TiC particle mixing enhanced aluminum-based composite material and preparation process thereof - Google Patents

In-situ SiC-TiC particle mixing enhanced aluminum-based composite material and preparation process thereof Download PDF

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CN102899517A
CN102899517A CN2012103722443A CN201210372244A CN102899517A CN 102899517 A CN102899517 A CN 102899517A CN 2012103722443 A CN2012103722443 A CN 2012103722443A CN 201210372244 A CN201210372244 A CN 201210372244A CN 102899517 A CN102899517 A CN 102899517A
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briquetting
situ
sic
preparation
tic particle
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CN102899517B (en
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梁艳峰
董晟全
李高宏
杨通
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Xian Technological University
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Xian Technological University
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Abstract

The invention relates to the technical field of non-continuous enhanced metal-based composite materials, and in particular relates to an in-situ SiC-TiC particle mixing enhanced aluminum-based composite material and a preparation process thereof. For overcoming the defects of high preparation cost, complicated process and poor wettability and compatibility of particles and substrates in the prior art, the invention provides the in-situ SiC-TiC particle mixing enhanced aluminum-based composite material and the preparation process thereof. The preparation process comprises the following steps: firstly, preparing in-situ reaction system press cakes: dividing the designed press cakes into inner and outer layers, wherein the mass ratio of the inner layer to the outer layer is 3:10, and then pressing by a pressure machine; then, preparing Al-4.5Cu based alloy by taking pure Al and Al-50% Cu as raw materials; and finally adding the press cakes in Al-4.5Cu melt to carry out in-situ reaction. Compared with the prior art, the preparation method disclosed by the invention has the advantages that the in-situ produced SiC particles are fine and reach micron scale.

Description

Original position SiC-TiC particle hybrid composite and preparation technology thereof
Technical field:
The present invention relates to Discontinuous Reinforcement metal-base composites technical field, be specifically related to a kind of original position SiC-TiC particle hybrid composite and preparation technology thereof.
Background technology:
Particle reinforced aluminium-based (the SiC of SiC p/ Al) matrix material is that recent two decades comes the worldwide the widest class Discontinuous Reinforcement metal-base composites of with fastest developing speed, application prospect.This matrix material has the good mechanical and physical characters such as specific tenacity height, specific modulus are high, high temperature resistant, wear-resistant, good stability of the dimension, the isotropic advantage of tool again, thereby be considered to a kind of desirable lightweight structural material, especially in the critical products such as motor vehicle engine piston, cylinder cylinder cap, cylinder body and aircraft industry, have broad application prospects.About the particle reinforced aluminium-based (SiC of SiC p/ Al) composite manufacture technique, modal is to adopt liquid forming, concrete grammar is to adopt stirring casting method.The SiC particle that is about to anticipate joins by churned mechanically method in the molten aluminium of melting, melt is carried out cast obtains as cast condition matrix material sample after the refining degasification.The shortcoming of this method has: the size of (1) SiC particle (mostly being 50-100 μ m) bigger than normal; (2) generally need to carry out pre-treatment to the SiC particle surface; (3) to equipment having relatively high expectations of mechanical stirring device particularly, otherwise the SiC particle is reunited in matrix material seriously; (4) add a little less than the poor interface binding power that causes the two of wetting property between SiC particle and the Al matrix, easily surface reaction is occuring at the interface, generate Al 3Ti or Al 4C 3Etc. harmful phase.
In-situ particle strengthens metal-base composites because have the advantage that particle is thinner, the interface combination is stronger, few to equipment requirements and impurity is few, becomes a kind of advanced composite material that develops rapidly in recent years.The preparation that in-situ particle strengthens metal-base composites mainly is to adopt the original position synthetic technology, ultimate principle is under certain condition, rely on design of alloy, by chemical reaction occurs in aluminium alloy, the pottery or the intermetallic compound that generate one or more high rigidity, high elastic coefficient strengthen body and reach the purpose that strengthens metallic matrix.The in-situ particle that adopts at present castmethod successfully to prepare strengthens metal-base composites and strengthens body with TiB 2With TiC be main.But with TiB 2, ceramic particle is diverse is for TiC etc., the SiC particle is difficult to directly use by means of the in-situ techniques of chemical reaction synthesize, this be because between Si and the C with stronger covalent bonds, aluminium liquid is difficult to wetting carbon, need higher energy because in alloy melt, directly synthesize SiC by chemical reaction simultaneously, therefore cause its preparation very difficult.Also do not see at present the relevant report that adopts the conventional cast method to prepare original position SiC particle enhanced aluminum-based composite material.
Summary of the invention:
The present invention will provide a kind of original position SiC-TiC particle hybrid composite and preparation technology thereof, preparation cost height, complex process, particle and the matrix wettability and the poor shortcoming of consistency that exist to overcome prior art.
The problem that exists in order to overcome prior art, technical scheme provided by the invention is:
A kind of preparation technology preparation technology of original position SiC-TiC particle hybrid composite is divided into two steps:
(1) preparation of in situ reaction system briquetting:
Under the condition that Ti:C=1:1, Si:C=1:1 (mol ratio) are constant in the design briquetting, briquetting is divided into inside and outside two-layer, titanium valve and Graphite Powder 99 mixture are as the skin of briquetting, silica flour and Graphite Powder 99 mixture are as the internal layer of briquetting, and outer and internal layer mass ratio is prepared by 3:10, suppresses at pressing machine, pressure is 20MPa, dwell time is 5 minutes, and compacting is taken out briquetting after finishing from mould, and it is dry to put into loft drier;
(2) select pure Al, Al-50%Cu is preparation of raw material Al-4.5Cu matrix alloy, put into plumbago crucible, heat fused, at 1000 ℃ briquetting joined and to carry out reaction in-situ in the Al-4.5Cu alloy melt, and be pressed into melt inside with graphite rod, the briquetting quality accounts for the 3-5wt.% of matrix alloy quality, question response stirs after finishing.Be cooled to 750 ℃ and use C 2Cl 6Carry out refinery by de-gassing, leave standstill 15-20min after, pour in the metal stretching coupon model at 720 ℃, naturally cooling namely makes as cast condition in-situ composite coupon; Matrix material 535 ± 5 ℃ of insulations 9 hours, is taken out and places at once 60~100 ℃ of quenching-in waters, carry out 5 hours ageing treatment at 175 ± 5 ℃ again.
The original position SiC-TiC particle hybrid composite that the above-mentioned preparation technology of a kind of usefulness makes.
The present invention adopts the reaction in-situ technology successfully to prepare original position SiC particle and TiC particle hybrid composite, prepared matrix material and the particle reinforced aluminium-based (SiC of traditional Si C p/ Al) matrix material is compared, and its advantage is:
(1) with add the SiC particle and prepare the SiC reinforced aluminum matrix composites and compare, generated in-situ SiC particle is more tiny, can reach submicron order;
(2) by to the design of the composition and structure of in situ reaction system, utilize titanium valve and Graphite Powder 99 to generate TiC institute liberated heat and compensate weak thermopositive reaction between Si and the C, adopt castmethod to obtain original position SiC particle.SiC delivers a child at the matrix alloy internal direct by chemical reaction, and therefore saved and anticipated, and good with the wetting property of matrix, the interface is in conjunction with stronger;
(3) SiC delivers a child at the matrix alloy internal direct by chemical reaction, only relies on the stirring of manual graphite rod can realize being evenly distributed, and very low to equipment requirements, common high temperature melting furnace can satisfy the preparation requirement.
Be evenly distributed during (4) because of reaction, SiC particle and Al matrix phase capacitive are good, and generated in-situ SiC particle is difficult for and Al matrix generation surface reaction, so seldom occurs Al in the microstructure of composite 3Ti or Al 4C 3
Description of drawings:
Fig. 1 is the structural representation of briquetting;
Fig. 2 is the metallographic structure figure of the prepared matrix material of embodiment 2;
Fig. 3 is the room temperature tensile port SEM shape appearance figure of the prepared matrix material of embodiment 2;
Fig. 4 is SiC particle and TiC particle TEM shape appearance figure in the prepared matrix material of embodiment 2;
Fig. 5 is SiC diffraction pattern figure in the prepared matrix material of embodiment 2;
Fig. 6 is TiC diffraction pattern figure in the prepared matrix material of embodiment 2.
Embodiment:
Below in conjunction with embodiment the present invention is described in detail.
Embodiment 1,
Be that ground and mixed is even in mortar for 1 silica flour (99% purity, 200 orders) and Graphite Powder 99 (99% purity, 200 orders) with mol ratio; Be that ground and mixed is even in mortar for 1 titanium valve (99% purity, 200 orders) and Graphite Powder 99 (99% purity, 200 orders) with mol ratio.Referring to Fig. 1, it is 35 millimeters moulds that two kinds of mixed powders are put into diameter, titanium valve and Graphite Powder 99 mixture are as the skin of briquetting, silica flour and Graphite Powder 99 mixture are as the internal layer of briquetting, outer mass ratio with internal layer is that 3:10(mediates silica flour and Graphite Powder 99 mixture, is the mixture of titanium valve and Graphite Powder 99 on every side).Briquetting is suppressed at pressing machine.Pressure is 20MPa, and the dwell time is 5 minutes.Compacting is taken out briquetting after finishing from mould, it is dry to put into loft drier.
Select pure Al ingot, the Al-50%Cu intermediate alloy ingot is preparation of raw material Al-4.5Cu matrix alloy, puts into plumbago crucible, heat fused at 1000 ℃, is pressed into melt inside with graphite rod with 3wt.% briquetting (the briquetting quality accounts for the 3wt.% of matrix alloy quality), question response stirs after finishing.Be cooled to 750 ℃ and use C 2Cl 6Carry out refinery by de-gassing, leave standstill 15min after, pour in the metal stretching coupon model at 720 ℃, naturally cooling namely makes as cast condition in-situ composite coupon; Matrix material 535 ± 5 ℃ of insulations 9 hours, is taken out and places at once 60 ℃ of quenching-in waters, carry out 5 hours ageing treatment at 175 ± 5 ℃ again.
The room temperature tensile the performance test results: tensile strength reaches 406MPa, and unit elongation reaches 11.3%;
Embodiment 2,
Be that ground and mixed is even in mortar for 1 silica flour (99% purity, 200 orders) and Graphite Powder 99 (99% purity, 200 orders) with mol ratio; Be that ground and mixed is even in mortar for 1 titanium valve (99% purity, 200 orders) and Graphite Powder 99 (99% purity, 200 orders) with mol ratio.It is 35 millimeters moulds that two kinds of mixed powders are put into diameter, titanium valve and Graphite Powder 99 mixture are as the skin of briquetting, silica flour and Graphite Powder 99 mixture are as the internal layer of briquetting, outer mass ratio with internal layer is that 3:10(mediates silica flour and Graphite Powder 99 mixture, is the mixture of titanium valve and Graphite Powder 99 on every side).Briquetting is suppressed at pressing machine.Pressure is 20MPa, and the dwell time is 5 minutes.Compacting is taken out briquetting after finishing from mould, it is dry to put into loft drier.Select pure Al ingot, the Al-50%Cu intermediate alloy ingot is preparation of raw material Al-4.5Cu matrix alloy, put into plumbago crucible, heat fused, at 1000 ℃, with graphite rod 5wt.% briquetting ((the briquetting quality accounts for the 5wt.% of matrix alloy quality)) is pressed into melt inside, question response stirs after finishing.Be cooled to 750 ℃ and use C 2Cl 6Carry out refinery by de-gassing, leave standstill 20min after, pour in the metal W tensile test bar model at 720 ℃, naturally cooling namely makes as cast condition in-situ composite coupon; Matrix material 535 ± 5 ℃ of insulations 9 hours, is taken out and places at once 60 ℃ of quenching-in waters, carry out 5 hours ageing treatment at 175 ± 5 ℃ again.
The room temperature tensile the performance test results: tensile strength reaches 428MPa, and unit elongation reaches 8.9%.
In the metallographic structure figure of the matrix material that embodiment 2 is prepared, room temperature tensile port SEM shape appearance figure, the matrix material in SiC particle and TiC particle TEM shape appearance figure, the matrix material in SiC diffraction pattern figure, the matrix material TiC diffraction pattern figure referring to Fig. 1-Fig. 6.

Claims (2)

1. the preparation technology of an original position SiC-TiC particle hybrid composite, described preparation technology is divided into two steps:
1) preparation of in situ reaction system briquetting:
Under the condition that Ti:C=1:1, Si:C=1:1 (mol ratio) are constant in the design briquetting, briquetting is divided into inside and outside two-layer, titanium valve and Graphite Powder 99 mixture are as the skin of briquetting, silica flour and Graphite Powder 99 mixture are as the internal layer of briquetting, and outer and internal layer mass ratio is prepared by 3:10, suppresses at pressing machine, pressure is 20MPa, dwell time is 5 minutes, and compacting is taken out briquetting after finishing from mould, and it is dry to put into loft drier;
2) select pure Al, Al-50%Cu is preparation of raw material Al-4.5Cu matrix alloy, put into plumbago crucible, heat fused, at 1000 ℃ briquetting joined and to carry out reaction in-situ in the Al-4.5Cu alloy melt, and be pressed into melt inside with graphite rod, the briquetting quality accounts for the 3-5wt.% of matrix alloy quality, after question response finishes, stir, be cooled to 750 ℃ and carry out refinery by de-gassing with C2Cl6, after leaving standstill 15-20min, pour in the metal stretching coupon model at 720 ℃, naturally cooling namely makes as cast condition in-situ composite coupon; Matrix material 535 ± 5 ℃ of insulations 9 hours, is taken out and places at once 60~100 ℃ of quenching-in waters, carry out 5 hours ageing treatment at 175 ± 5 ℃ again.
2. original position SiC-TiC particle hybrid composite that the preparation technology who utilizes a kind of original position SiC-TiC particle hybrid composite claimed in claim 1 makes.
CN201210372244.3A 2012-09-29 2012-09-29 In-situ SiC-TiC particle mixing enhanced aluminum-based composite material and preparation process thereof Expired - Fee Related CN102899517B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104141063A (en) * 2014-07-31 2014-11-12 重庆大学 Preparing method of in-situ synthesis titanium carbide enhanced titanium-based multi-hole materials
CN109182802A (en) * 2018-11-12 2019-01-11 华北电力大学(保定) A kind of carbon material enhancing copper/aluminum matrix composite preparation method
CN112692295A (en) * 2020-12-11 2021-04-23 迈特李新材料(深圳)有限公司 Aluminum-based nano composite material powder for 3D printing and preparation method thereof
CN114318435A (en) * 2021-12-31 2022-04-12 西安工业大学 Aluminum-based composite material with internal stress adjusting function 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
CN104141063A (en) * 2014-07-31 2014-11-12 重庆大学 Preparing method of in-situ synthesis titanium carbide enhanced titanium-based multi-hole materials
CN104141063B (en) * 2014-07-31 2015-12-09 重庆大学 A kind of fabricated in situ titanium carbide strengthens the preparation method of titanium based porous materials
CN109182802A (en) * 2018-11-12 2019-01-11 华北电力大学(保定) A kind of carbon material enhancing copper/aluminum matrix composite preparation method
CN112692295A (en) * 2020-12-11 2021-04-23 迈特李新材料(深圳)有限公司 Aluminum-based nano composite material powder for 3D printing and preparation method thereof
CN112692295B (en) * 2020-12-11 2021-09-10 迈特李新材料(深圳)有限公司 Aluminum-based nano composite material powder for 3D printing and preparation method thereof
CN114318435A (en) * 2021-12-31 2022-04-12 西安工业大学 Aluminum-based composite material with internal stress adjusting function and preparation method thereof
CN114318435B (en) * 2021-12-31 2023-08-29 西安工业大学 Aluminum-based composite material with internal stress adjusting function and preparation method thereof

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