CN100357468C - Preparation method of endogenous particle reinforced aluminium-based composite material - Google Patents
Preparation method of endogenous particle reinforced aluminium-based composite material Download PDFInfo
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- CN100357468C CN100357468C CNB2005100387068A CN200510038706A CN100357468C CN 100357468 C CN100357468 C CN 100357468C CN B2005100387068 A CNB2005100387068 A CN B2005100387068A CN 200510038706 A CN200510038706 A CN 200510038706A CN 100357468 C CN100357468 C CN 100357468C
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- 239000002245 particle Substances 0.000 title claims abstract description 32
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000004411 aluminium Substances 0.000 title claims description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000005516 engineering process Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000005266 casting Methods 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 230000006698 induction Effects 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000000956 alloy Substances 0.000 claims description 16
- 229910045601 alloy Inorganic materials 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000007872 degassing Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000009749 continuous casting Methods 0.000 claims description 8
- 238000007670 refining Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000005672 electromagnetic field Effects 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 4
- 238000005457 optimization Methods 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 229910006501 ZrSiO Inorganic materials 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000155 melt Substances 0.000 abstract description 3
- 238000013019 agitation Methods 0.000 abstract 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000005728 strengthening Methods 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 22
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000008187 granular material Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- 229910001338 liquidmetal Inorganic materials 0.000 description 3
- 238000005551 mechanical alloying Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- DRLFMBDRBRZALE-UHFFFAOYSA-N melatonin Chemical compound COC1=CC=C2NC=C(CCNC(C)=O)C2=C1 DRLFMBDRBRZALE-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 208000035126 Facies Diseases 0.000 description 1
- 240000003936 Plumbago auriculata Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007582 slurry-cast process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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Abstract
The present invention has the purpose of providing a method for preparing an endogenic particle strengthened aluminum-based composite material in industrial scale preparation, namely a melt reaction method, electromagnetic agitation processing and an integrated technology for D. C. casting forming. The method comprises the steps that a compound containing strengthened particle forming elements is added to fused aluminum or aluminum alloy at certain temperature, and simultaneously, electromagnetic agitation is applied to cause the compound to sufficiently react, and endogenic particles are uniformly distributed in the melt to obtain a composite material melt and then form a bar by D. C. casting. Therefore, the present invention has the advantages of simple technology, low cost, short period, satisfaction of industrial production, etc. and is one of new technologies for realizing the industrial scale production and the application of endogenic particle strengthened aluminum-based composite materials. The endogenic particles prepared by the method not only have high strength, high hardness and high elastic modulus, but also have small grain size (the average diameter of the endogenic particles is less than or equal to 2 um) and are uniformly distributed in a basal body so as to have favorable strengthening effect.
Description
Technical field
The present invention relates to a kind of preparation method of endogenous particle reinforced aluminium-based composite material, promptly it is integrated by melting-reaction method+induction stirring processing+semi-continuous casting.
Background technology
Endogenetic particle strengthens metal matrix (aluminium base) matrix material because to strengthen body be original position forming core, the thermodynamically stable phase of growing up from metallic matrix (being generally Al), therefore, it is pollution-free to strengthen the surface, has avoided the problem bad with the matrix consistency, and the interface bond strength height.Thereby be described as and have breakthrough NEW TYPE OF COMPOSITE and extremely pay attention to, become a new focus in the research of metal matrix (particularly aluminium base) matrix material in recent years.According to participating in the state difference that synthetic two reactive components that strengthen body exist, Gu this technology mainly can be divided into solution-air, solid-liquid, solid-etc. three kinds of reaction patterns.
(1) gas-liquid reaction method (VLS method):
This method is by people such as M J Koczak invention and declared United States Patent (USP).Its technological principle is that the employing rare gas element is a carrier, the gas that will contain C or N feeds in the superalloy liquid, make C or the reaction of the individual components in N and the alloy liquid in the decomposing gas, in alloy substrate, form the stable high rigidity of tiny disperse, the carbide or the nitride of high elastic coefficient, generate thermodynamically stable ceramic particle enhanced metal-base composites after the cooled and solidified.
(2) solid-liquid reaction method
The Lanxide method is by the exploitation of U.S. Lanxide company, and it is by metal direct oxidation method (DIMOX
TM) and metal pressure-free impregnation method (PRIMEX
TM) both form.DIMOX
TMMethod allows metal and alloy thereof carry out the ceramic metal based composites that direct oxidation prepares certain component under melting condition.Operational path has two kinds, and a kind of is that ceramic particle and whisker are cold-pressed into base, puts into aluminium liquid then, at high temperature generates Al with oxygen
2O
3Second kind is ceramic particle and aluminium to be mixed carry out slurry casting moulding Al oxidation and growth in the ceramic particle gap.
PRIMEX
TMMethod, different with DIMOX what be to use is non-oxidizing gas, in this technology, two processes takes place simultaneously: the one, liquid metal is the infiltration in ceramics preparative spare under the effect of ambiance; The 2nd, the reaction of liquid metal and surrounding gas and generate new enhancing particle.Discover that the quantity of the AlN that original position forms and size depend primarily on the wetting-out rate of Al liquid, and N in the wetting-out rate of Al liquid and the ambiance
2The temperature of dividing potential drop, melt is relevant with composition, and therefore, the tissue of matrix material and performance are easily by adjusting composition, the N of melt
2Dividing potential drop and treatment temp and being controlled effectively.
XD
TMMethod: this technology is by U.S.'s Martin Marietta laboratory invention.It is with two solid-state reactive element powder and metallic matrix powder mixes evenly and after the compacting degasification, and pressed compact is heated rapidly to temperature more than the metallic matrix fusing point, and heat-producing chemical reaction takes place in melt the reagent element, generates the wild phase ceramic particle.Prepare matrix material with this Technology, wild phase is wetting by liquid metal, and the interface is just becoming a focus of current matrix material research in conjunction with firmly.But too tiny particle can significantly increase the viscosity of melt, is difficult to further casting.
(3) solid-solid reaction method
Mechanical alloying method: MA (Mechanical Alloying) technology is the new and high technology of preparation powdered alloy, and with different powder ball milling in high energy ball mill, powder deforms through extruding, diffusion or carry out solid state reaction and form alloy between atom.
But method for preparing technology and equipment complexity, and cost height are difficult to realize commercial scale production and application.
Summary of the invention
Preparation method-melting-reaction method+induction stirring processing+semi-continuous casting the integrated technology that the objective of the invention is a kind of endogenous particle reinforced aluminium-based composite material.This method is that the compound that will contain the enhanced granule forming element joins in the fused aluminum or aluminum alloy under a certain temperature, apply induction stirring simultaneously, make it abundant reaction, and make endogenetic particle distribution uniform in melt, the Composite Melt that obtains becomes bar through D.C.casting.
Technical scheme of the present invention is:
It is characterized in that adopting melting-reaction method+induction stirring processing+semi-continuous casting integrated technology to prepare particle enhanced aluminum-based composite material, mainly comprise the optimization and integrated technology two aspects of reaction system:
(1) optimization of reaction system
Reaction system is made up of molten aluminium and the compound that contains the particle forming element, and they can be one of following assembled schemes:
①Al-ZrSiO
4；
②Al-TiO
2-KBF
4；
③Al-K
2TiF
6-KBF
4；
④Al-ZrOCl
2；
⑤Al-Zr(CO
3)
2-B
2O
3。
With reactant mixing by a certain percentage, stay with stand-by;
(2) integrated technology
Fine aluminium or its alloy are melted in the pottery of electrical induction heating device or plumbago crucible, and Heating temperature is above 200～300 ℃ of this alloy melting point; Reactant is according to a certain ratio added in the aluminium liquid by conduit, carry out induction stirring with the electromagnetism stirrer simultaneously, react fully and carry out, reaction still need apply induction stirring 5min after finishing, and the reaction times, view volume system was different and different, finished in 40min usually; The strength of current that stirs is 30～50 amperes, and electromagnetic field frequency is 5～20Hz; Be incubated in the time of reaction, holding temperature is above 150～200 ℃ of this alloy liquid phase line, and the slagging-off of reaction back is carried out the nitrogen degasification, refining time 10～15 minutes; Melt temperature carries out D.C.casting during for above 150～200 ℃ of this alloy liquid phase line and becomes bar.
The invention has the advantages that technology is simple, cost is low, the cycle is short, satisfy suitability for industrialized production, is one of new technology that realizes endogenous granular reinforced aluminum base composite material commercial scale production and application.The endogenetic particle of this method preparation not only has high intensity, consistency and elasticity modulus, and the little (mean diameter≤2um), and being evenly distributed in matrix, thereby reinforced effects is good of particle size.
The present invention is integrated in particle enhanced aluminum-based composite material with fusant reaction synthetic technology and electromagnetic agitating technology and semi-continuous casting technology, thereby the size and the distribution of control endogenetic particle obtain the stable and ideal endogenous granular reinforced aluminum base composite material comparatively of tissue.
Description of drawings
For for a more detailed description, existing as follows with the figure brief introduction in conjunction with the embodiments to the present invention:
Fig. 1 the present invention prepares particle enhanced aluminum-based composite material device synoptic diagram;
The matrix material facies analysis figure of Fig. 2 the present invention preparation
The matrix material micro-organization chart of Fig. 3 embodiment 1
The matrix material micro-organization chart of Fig. 4 embodiment 2
The matrix material micro-organization chart of Fig. 5 embodiment 3
1 thermopair, 2 metal melts, 3 ceramic crucibles, 4 induction stirring machines, 5 resistance furnaces, 6 thermopairs, 7 conduits
Embodiment
Embodiment 1: heating resistor stove (5), commercial-purity aluminium is melted in ceramic crucible (3), be superheated to 950 ℃ of insulations, carry out nitrogen degasification refining, and after leaving standstill 12min, with account for aluminium liquid mass percent 7.6% ZrSiO
4Pulvis adds in the molten aluminium by conduit (7), and use electromagnetism stirrer (4) to begin to carry out induction stirring simultaneously, be incubated simultaneously, induction stirring electric current 30A, electromagnetic field frequency 10Hz, churning time 40min, nitrogen degasification refining 10min is carried out in slagging-off more then, carries out semi-continuous casting in the time of 800 ℃.Give birth to (Al in this matrix material
3Zr+Al
2O
3) the theoretical volume mark of enhanced granule is 5%.Fig. 3 is the micro-organization chart of this matrix material, and as seen from Figure 3, the particle of generation is tiny.
Embodiment 2: heating resistor stove (5), the A356 alloy is melted in ceramic crucible (3), and be superheated to 900 ℃ of insulations, carry out nitrogen degasification refining, and after leaving standstill 15min, will account for the pulvis ZrOCl of molten aluminium alloy mass percent 13.1%
2Join in the molten aluminium alloy by conduit (7), and use electromagnetism stirrer (4) to begin to carry out induction stirring simultaneously, be incubated simultaneously, induction stirring electric current 40A, electromagnetic field frequency 15Hz, churning time 30min, nitrogen degasification refining 12min is carried out in slagging-off more then, carries out semi-continuous casting in the time of 800 ℃.Give birth to (Al in this matrix material
3Zr+Al
2O
3) the theoretical volume mark of enhanced granule is 10%.As seen from Figure 4, the particle of generation is tiny.
Embodiment 3: heating resistor stove (5), the A356 alloy is melted in ceramic crucible (3), and be superheated to 900 ℃ of insulations, carry out nitrogen degasification refining, and after leaving standstill 15min, will account for the mixing powder (K of matrix alloy liquid mass percent 21.4%
2TiF
6+ KBF
4) by Ti: B=1: 2 molar ratio mixes by conduit (7) and joins in the molten aluminium alloy, and use electromagnetism stirrer (4) to begin to carry out induction stirring simultaneously, be incubated simultaneously, induction stirring electric current 50A, electromagnetic field frequency 20Hz, churning time 25min, nitrogen degasification refining 15min is carried out in slagging-off more then, carries out semi-continuous casting in the time of 800 ℃.Give birth to (TiB in this matrix material
2+ Al
3Ti) the theoretical volume mark of enhanced granule is 15%.As seen from Figure 5, the particle of generation is tiny.
Table 1 is the mechanical property with the part matrix material that comprises embodiment 1,2,3 of this integrated technology preparation.
Table 1
| Material | Tensile strength sigma b/MPa | Unit elongation δ/% | Hardness HB | |
| 5％vol(Al 3Zr+Al 2O 3)p/Al | 113.5 | 34.3 | 47.6 | As cast condition |
| 10％vol(Al 3Zr+Al 2O 3)p/Al | 152.4 | 28.4 | 58.4 | As cast condition |
| 15％vol(Al 3Zr+Al 2O 3)p/Al | 246.7 | 12.5 | 69.2 | As |
| 5％vol(Al 3Zr+Al 2O 3)p/A356 | 255.7 | 9.6 | 84.6 | |
| 5％vol(Al 3Zr+Al 2O 3)p/A356 | 289.8 | 11.4 | 88.4 | T6 |
| 10％vol(Al 3Zr+Al 2O 3)p/A356 | 307.5 | 8.8 | 89.2 | As cast condition |
| 10％vol(Al 3Zr+Al 2O 3)p/A356 | 354.5 | 9.3 | 98.7 | T6 |
| 15％vol(Al 3Zr+Al 2O 3)p/A356 | 386.8 | 5.6 | 104.5 | As cast condition |
| 15％vol(Al 3Zr+Al 2O 3)p/A356 | 401.4 | 6.8 | 110.6 | |
| 5％vol(TiB 2+Al 3Ti)p/Al | 115.5 | 33.4 | 45.7 | As cast condition |
| 10％vol(TiB 2+Al 3Ti)p/Al | 158.7 | 26.4 | 56.9 | As cast condition |
| 15％vol(TiB 2+Al 3Ti)p/Al | 212.6 | 12.8 | 66.8 | As |
| 5％vol(TiB 2+Al 3Ti)p/A356 | 254.3 | 10.4 | 83.8 | As |
| 5％vol(TiB 2+Al 3Ti)p/A356 | 286.6 | 11.8 | 86.8 | T6 |
| 10％vol(TiB 2+Al 3Ti)p/A356 | 318.5 | 8.2 | 88.7 | As cast condition |
| 10％vol(TiB 2+Al 3Ti)p/A356 | 348.7 | 9.1 | 98.9 | T6 |
| 15％vol(TiB 2+Al 3Ti)p/A356 | 388.7 | 6.8 | 102.6 | As cast condition |
| 15％vol(TiB 2+Al 3Ti)p/A356 | 412.9 | 7.2 | 108.7 | T6 |
Claims (1)
1. the preparation method of an endogenous particle reinforced aluminium-based composite material, it is characterized in that adopting melting-reaction method+induction stirring processing+semi-continuous casting integrated technology to prepare particle enhanced aluminum-based composite material, comprise the optimization and integrated technology two aspects of reaction system:
(1) optimization of reaction system
Reaction system is made up of molten aluminium and the compound that contains the particle forming element, and they are one of following assembled schemes:
①Al-ZrSiO
4；
②Al-TiO
2-KBF
4；
③Al-K
2TiF
6-KBF
4；
④Al-ZrOCl
2；
⑤Al-Zr(CO
3)
2-B
2O
3；
Reactant is mixed to evenly by a certain percentage, stays with stand-by;
(2) integrated technology
Fine aluminium or its alloy are melted in the ceramic crucible of electrical induction heating device, and Heating temperature is above 200～300 ℃ of this alloy melting point; Reactant is according to a certain ratio added in the aluminium liquid by conduit, carry out induction stirring with the electromagnetism stirrer simultaneously, react fully and carry out, reaction still need apply induction stirring 5min after finishing, and the reaction times, view volume system was different and different, finished in 40min usually; The strength of current that stirs is 30～50 amperes, and electromagnetic field frequency is 5～20Hz; Be incubated in the time of reaction, holding temperature is above 150～200 ℃ of this alloy liquid phase line, and the slagging-off of reaction back is carried out the nitrogen degasification, refining time 10～15 minutes; Melt temperature carries out D.C.casting during for above 150～200 ℃ of this alloy liquid phase line and becomes bar.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100387068A CN100357468C (en) | 2005-04-05 | 2005-04-05 | Preparation method of endogenous particle reinforced aluminium-based composite material |
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| Publication Number | Publication Date |
|---|---|
| CN1667147A CN1667147A (en) | 2005-09-14 |
| CN100357468C true CN100357468C (en) | 2007-12-26 |
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Cited By (1)
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|---|---|---|---|---|
| RU2729267C1 (en) * | 2020-01-20 | 2020-08-05 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Тихоокеанский государственный университет" | Method of producing cast composite aluminum matrixed alloys |
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| CN1944699B (en) * | 2006-07-14 | 2010-05-12 | 江苏大学 | High volume fractional endogenous granular reinforced aluminum base composite material and its preparing method |
| CN100577831C (en) * | 2007-11-23 | 2010-01-06 | 中国铝业股份有限公司 | Apparatus for industrialized preparation of granule-reinforced aluminium-based composite material |
| CN101880783B (en) * | 2010-06-03 | 2012-02-08 | 南昌大学 | Preparation method of TiAl3 enhanced aluminum-based composite material |
| CN101892406B (en) * | 2010-07-15 | 2012-06-20 | 江苏大学 | Method for preparing aluminum-based composite material with uniform and fine isometric crystal grains |
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| CN102994822A (en) * | 2012-11-20 | 2013-03-27 | 江苏大学 | Preparation method for generating low-expansion coefficient aluminum matrix composite by using magnetochemistry |
| CN102994814A (en) * | 2012-11-22 | 2013-03-27 | 江苏大学 | Mixed particle reinforced wear-resisting aluminum matrix composite which is generated in-situ in magnetic field and preparation method thereof |
| CN106350694A (en) * | 2016-08-25 | 2017-01-25 | 上海交通大学 | Method for continuously preparing in-situ particle-reinforced aluminum matrix composite |
| CN109797318B (en) * | 2019-04-01 | 2021-08-20 | 重庆大学 | Preparation of Al3Method for Ti reinforcing aluminum-based material |
| CN114318067B (en) * | 2021-12-23 | 2023-01-03 | 南京理工大学 | Multi-carbide particle reinforced aluminum matrix composite and preparation method thereof |
| CN114318025B (en) * | 2021-12-23 | 2022-06-21 | 中南大学 | Bimetal liquid phase in-situ smelting device |
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| GB2259309A (en) * | 1991-09-09 | 1993-03-10 | London Scandinavian Metall | Ceramic particles |
| JP2000005852A (en) * | 1998-06-23 | 2000-01-11 | Furukawa Electric Co Ltd:The | Cracking prevention device for aluminum alloy ingot, and dc casting method |
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-
2005
- 2005-04-05 CN CNB2005100387068A patent/CN100357468C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2259309A (en) * | 1991-09-09 | 1993-03-10 | London Scandinavian Metall | Ceramic particles |
| JP2000005852A (en) * | 1998-06-23 | 2000-01-11 | Furukawa Electric Co Ltd:The | Cracking prevention device for aluminum alloy ingot, and dc casting method |
| CN1490428A (en) * | 2003-08-29 | 2004-04-21 | 东北大学 | Method and apparatus for preparing aluminium base composite materials under high magnetic field |
Non-Patent Citations (1)
| Title |
|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2729267C1 (en) * | 2020-01-20 | 2020-08-05 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Тихоокеанский государственный университет" | Method of producing cast composite aluminum matrixed alloys |
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