CN1470662A - Method for preparing two-phase granular mixed reinforced magnesium alloy based composite material - Google Patents
Method for preparing two-phase granular mixed reinforced magnesium alloy based composite material Download PDFInfo
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Abstract
The new process for preparing TiB2 and TiC double-phase mixed hybridization reinforced magnesium alloy base composite material is characterized by that it adopts Al-Ti-B-C system reaction prefabricated block and makes it produce chemical synthesis reaction under the condition of vacuum or inert gas protection to prepare (TiB2+TiC)/Al intermediate phase carrier, then adds the intermediate phase carrier into molten magnesium alloy to make dissolution and diffusion, and fully stirs them to make said intermediate phase carrier be uniformly distributed in molten magnesium alloy to obtain the invented product in which the TiB2 is formed into block form and the TiC is formed into ball form, so that the comprehensive performance of said composite can be obviously raised.
Description
Technical field
The present invention relates to the preparation method of magnesium alloy composite, particularly relate to the preparation method that biphase confusion strengthens the magnesium alloy composite of mode.
Background technology
Composite material of magnesium alloy more and more receives the concern in automobile, aerospace field owing to have excellent comprehensive performances such as light weight, specific tenacity height, wear resistance and high-temperature behavior are good.At present, the enhancing mode of magnesium alloy composite mainly contains fiber reinforcement and particle and strengthens two kinds.Because the fiber reinforcement complex process, the cost height, poor with the matrix wettability, and shortcoming such as continuous fibre enhanced machining property difference, limited the promotion and application of alloy fiber reinforced magnesium based composites greatly, be difficult to realize the mass-producing commercial production.Directly add particle and strengthen mode, because adding particle surface is polluted easily, therefore wild phase and matrix wettability are poor, cause the interface of enhanced granule and matrix bad, a series of problems such as surface reaction easily take place, and particle is generally all thicker, is easy to gather partially in crystal boundary, thereby reinforced effects is undesirable, and is more with the research of SiC granule reinforced magnesium alloy-base composite material in this method.
In addition, also have two kinds of emerging technologies among the preparation method of granule reinforced magnesium alloy-base composite material: a kind of is the prefabricated section that adopts the Al-Ti-C system, make the TiC/Al master alloy by self-propagating reaction, then this master alloy is joined in the magnesium alloy fused mass, thereby prepare TiC granule reinforced magnesium alloy-base composite material (Chinese patent application number: 02109102.1); Another is to adopt the Al-Ti-C system, or the prefabricated section of Al-Ti-C-Mg system, directly join in magnesium alloy fused mass through after the pre-treatment unreacted prefabricated section green compact, in the magnesium melt, react, thereby the interior ceramic particle TiC that give birth to form prepares TiC granule reinforced magnesium alloy-base composite material (Chinese patent application number 01128168.5 and 02132648.7).But, adopting that TiC often exists with the form of C omission in the matrix material of above-mentioned prepared, the TiC hardness of vacant form descends, and can not give full play to its reinforced effects; And if improper process control in the preparation process, generate fragility phase TiAl easily
3Thereby, cause performance of composites to descend.
Summary of the invention
It is simple relatively, reliable to the purpose of this invention is to provide a kind of technology, and the biphase confusion with good over-all properties that is easy to the mass-producing commercial production strengthens the preparation method of magnesium alloy composite.
Technical scheme of the present invention is: adopt Al-Ti-B-C system reaction prefabricated block to issue biochemical building-up reactions in vacuum or protection of inert gas, make (TiB
2+ TiC)/and the Al intermediate phase carrier, this intermediate phase carrier is joined dissolve diffusion in the magnesium alloy fused mass again, impel it to be uniformly distributed in the magnesium alloy fused mass through stirring, thereby prepare TiB
2Strengthen magnesium alloy composite with the TiC biphase confusion, its technological process comprise reaction prefabricated block preparation, contain two-phase and mix dissolving diffusion and the two-phase disperse that mixes enhanced granule in magnesium alloy fused mass of the preparation of intermediate phase carrier of enhanced granule and intermediate phase carrier and distribute.Its technological process is as follows:
1) preparation of reaction prefabricated block:
A. prefabricated section is formed: prefabricated section is by size range Al, Ti, C and four kinds of powder constituents of B at 0.5～80 micron, and Al powder content weight percent is 28～62%, atomic ratio (B+C): Ti=2.8～3.2,
B. batch mixing: the above-mentioned powder for preparing is packed in the ball mill, and ball milling 4～30 hours mixes,
C. compression moulding: the powder that mixes is put into mould, briquetting at room temperature, pressing block density is 60～88% of this mixed powder theoretical density;
2) contain the preparation that two-phase mixes the intermediate phase carrier of enhanced granule:
Reaction prefabricated block put into vacuum or the heating unit of high-purity argon protective atmosphere is arranged, be heated to 600～800 ℃ with the heating rate of 5～30 ℃/min, cause chemosynthesis reaction, reaction product is for containing enhanced granule TiB
2, TiC and Al intermediate phase carrier;
3) dissolving diffusion and the two-phase disperse that mix enhanced granule of intermediate phase carrier in magnesium alloy substrate distributes:
A. the melting of matrix alloy: the crucible that an amount of matrix magnesium alloy will be housed is put into resistance furnace and is heated, and for preventing the oxidizing fire of magnesium alloy in the fusion process, can adopt flux to be protected or high-purity argon gas is protected, and melt temperature remains on 690～850 ℃,
B. the dissolving diffusion of intermediate phase carrier in magnesium alloy substrate: press TiB
2The weight percent that+TiC accounts for the matrix material total amount is the quality that 2～16% amount calculates corresponding intermediate phase carrier, and this intermediate phase carrier is put into 690～850 ℃ magnesium alloy fused mass, treat to stir after its dissolving diffusion,
C. melt stirring technique: whipping temp is 590～700 ℃, and churning time is 15～60min, impels two-phase to mix enhanced granule TiB through stirring
2Be distributed in the magnesium alloy fused mass with the TiC even dispersion,
D. cast obtains TiB after the refining degasification
2Strengthen magnesium alloy composite with the TiC biphase confusion.
The present invention compares with present existing technology has following characteristics:
1) technology is simple, is easy to apply on producing.The invention is characterized in TiB
2Mixing enhanced granule with the TiC two-phase and generate in metallic aluminium through chemosynthesis reaction, because the fusing point of aluminium is low, is 660 ℃ only, is suitable for as intermediate carrier, and process stabilizing is reliable.Enhanced granule is tiny, and surface clean is pollution-free, and is good with the wettability of matrix, thereby combines well with basal body interface, thereby improved the over-all properties of matrix material.Overcome add the easily oxidation stain of enhanced granule surface, poor with the wettability of matrix, particle is generally all thicker and skewness and easily gathering in problems such as crystal boundaries partially.Metallic aluminium in the intermediate phase carrier is the main strengthening element of magnesium alloy, and bigger solid solubility is arranged in magnesium, so intermediate phase carrier is easy to dissolving diffusion, and after agitation as appropriate, wild phase is evenly distributed in matrix, and reinforced effects is remarkable.
2) two-phase that makes of the inventive method mixes TiB in the enhanced granule
2Size is about～and 3 microns, it is block that shape mostly is; The TiC size is about～and 1.5 microns, be shaped as closely spherical.Because TiB
2Has different lattice lattice structures with TiC, as TiB
2Be close-packed hexagonal structure, lattice parameter is a=3.03034, c=3.22953, and TiC is a face-centred cubic structure, lattice parameter a=3.33883, and different physicochemical property, all variant as density, hardness, the coefficient of expansion etc., therefore in the magnesium alloy substrate process of setting, have different effects.Therefore, biphase confusion strengthens magnesium alloy composite and both had been different from single-phase TiC granule reinforced magnesium alloy-base composite material, also is different from single-phase TiB
2The granule reinforced magnesium alloy-base composite material.The present invention can divide performance TiB
2Mix the advantage of enhanced granule with the TiC two-phase, significantly improve the over-all properties of matrix material.
3) biphase confusion of the inventive method preparation strengthens the TiB in the magnesium alloy composite
2Be evenly distributed in matrix with TiC, be difficult for producing segregation, and can carry out repeatedly remelting.
Description of drawings
Fig. 1 is intermediate phase carrier (50%TiB
2+ 10%TiC)/microcosmic of 40%Al scanning tissue
Fig. 2 is intermediate phase carrier (50%TiB
2+ 10%TiC)/X-ray diffraction analysis of 40%Al
Fig. 3 is matrix material 10% (TiB
2+ TiC)/microcosmic of AZ91 scanning tissue
Fig. 4 is matrix material 10% (TiB
2+ TiC)/X-ray diffraction analysis of AZ91
Fig. 5 is intermediate phase carrier (25%TiB
2+ 25%TiC)/microcosmic of 50%Al scanning tissue
Fig. 6 intermediate phase carrier (25%TiB
2+ 25%TiC)/X-ray diffraction analysis of 50%Al
Fig. 7 is matrix material 5% (TiB
2+ TiC)/microcosmic of AZ91 scanning tissue
Fig. 8 is matrix material 5% (TiB
2+ TiC)/X-ray diffraction analysis of AZ91
Embodiment
Embodiment 1
Produce 10% (TiB
2+ TiC)/the AZ91 matrix material
Get～29 microns Al powder ,～15 microns Ti powder ,～3 microns B powder and～38 microns C powder, the matrix magnesium alloy adopts AZ91 ingot, pure magnesium ingot and pure zinc, Al-Mn master alloy batching.Is 40% with above four kinds of powder by Al content weight percent, atomic ratio (B+C): Ti=3.0, and atomic ratio B: Ti=2, weight ratio B+Ti is 50% ratio, in the drum-type small grinder, mixed 8 hours, be pressed into the cylindrical reaction prefabricated block of φ 55 * 30 then on 20 tons of pressing machinees, the pressed compact compact rate of molding is 75% of a mixed powder theoretical density.Reaction prefabricated block is placed in the heating under vacuum device, is warming up to 680 ℃ with the heating rate of 10 ℃/min, cause chemosynthesis reaction, product is (50%TiB
2+ 10%TiC)/and the 40%Al intermediate phase carrier, its microcosmic scanning tissue and X-ray diffraction analysis are as shown in Figure 1 and Figure 2.To contain corresponding TiB then
2Add in 750 ℃ the liquid magnesium alloy that the high-purity argon gas protection is arranged with the intermediate phase carrier of TiC diphase particles, treat the intermediate phase carrier fusion after, be cooled to 620 ℃ and stir, churning time is 20min.After stirring finishes, be warming up to 750 ℃, the refining degasification pours in the metal type dies, makes 10% (TiB
2+ TiC)/and the AZ91 matrix material, its microcosmic scanning tissue and X-ray diffraction analysis are as shown in Figure 3, Figure 4.
Produce 15% (TiC+TiB
2)/ZM5 matrix material
Get～74 microns Al powder ,～25 microns Ti powder ,～3 microns B powder and～74 microns C powder, the matrix magnesium alloy adopts ZM5 ingot, pure magnesium ingot Al-Mn master alloy and pure zinc batching.Is 60% with above four kinds of powder by Al content weight percent, atomic ratio (B+C): Ti=3.1, and atomic ratio B: Ti=2, weight ratio B+Ti is 10%, in the drum-type small grinder, mixed 24 hours, be pressed into the cylindrical reaction prefabricated block of φ 55 * 30 then, the pressed compact compact rate of molding is 82% of a mixed powder theoretical density.Reaction prefabricated block is placed in the high-purity argon gas protection heating unit down, is warming up to 765 ℃ with the heating rate of 25 ℃/min, the initiation chemosynthesis reaction makes (30%TiC+10%TiB
2)/60%Al intermediate phase carrier contains this corresponding TiC and TiB subsequently
2The intermediate phase carrier that two-phase mixes ceramic particle adds to be had in 800 ℃ the liquid magnesium alloy of flux protection, treat the intermediate phase carrier fusion after, be cooled to 680 ℃ of stirrings, churning time is 40min.After stirring finishes, be warming up to 760 ℃, the refining degasification pours in the metal type dies, makes 15% (TiC+TiB
2)/ZM5 matrix material.Composite as-cast hardness is HB82, has improved 36% than the hardness of matrix AZ91 magnesium alloy; Wear resistance has improved 90% than the matrix magnesium alloy.
Embodiment 3
Produce 5% (TiB
2+ TiC)/the AZ91 matrix material
Get～29 microns Al powder ,～15 microns Ti powder ,～3 microns B powder ,～38 microns C powder, matrix magnesium alloy adopt AZ91HP ingot, pure magnesium ingot, Al-Mn master alloy and the preparation of pure zinc.Is 50% with above four kinds of powder by Al content weight percent, atomic ratio (B+C): Ti=3, and atomic ratio B: Ti=2, weight ratio B+Ti is 25% ratio, in the drum-type small grinder, mixed 16 hours, be pressed into the cylindrical reaction prefabricated block of φ 55 * 30 then on 20 tons of pressing machinees, the pressed compact compact rate of molding is 75% of a mixed powder theoretical density.Reaction prefabricated block is placed in the heating under vacuum device, is warming up to 640 ℃ with the heating rate of 18 ℃/min, cause chemosynthesis reaction, product is (25%TiB
2+ 25%TiC)/and the 50%Al intermediate phase carrier, its microcosmic scanning tissue and X-ray diffraction analysis such as Fig. 5, shown in Figure 6.Subsequently this is contained corresponding TiB
2Adding with the intermediate phase carrier of TiC diphase particles has in 700 ℃ the liquid magnesium alloy of flux protection, treat the intermediate phase carrier fusion after, be cooled to 650 ℃ and stir, churning time is 30min.After stirring finishes, be warming up to 780 ℃, the refining degasification pours in the metal type dies, makes 5% (TiB
2+ TiC)/and the AZ91 matrix material, its microcosmic scanning tissue and X-ray diffraction analysis such as Fig. 7, shown in Figure 8.
Embodiment 4
Produce 3% (TiB
2+ TiC)/the AM50 matrix material
Get～74 microns Al powder ,～15 microns Ti powder ,～3 microns B powder ,～0.5 micron C powder, matrix magnesium alloy adopt AM50 ingot, pure magnesium ingot, Al-Mn master alloy and the preparation of pure zinc.Is 60% with above four kinds of powder by Al content weight percent, atomic ratio (B+C): Ti=3.2, and atomic ratio B: Ti=2, weight ratio B+Ti is 35% ratio, in the drum-type small grinder, mixed 16 hours, be pressed into the cylindrical reaction prefabricated block of φ 55 * 30 then on 20 tons of pressing machinees, the pressed compact compact rate of molding is 75% of a mixed powder theoretical density.Reaction prefabricated block is placed in the heating under vacuum device, is warming up to 680 ℃ with the heating rate of 25 ℃/min, cause chemosynthesis reaction, product is (35%TiB
2+ 5%TiC)/the 60%Al intermediate phase carrier.Subsequently this is contained corresponding TiB
2Adding with the intermediate phase carrier of TiC diphase particles has in 750 ℃ the liquid magnesium alloy of flux protection, treat the intermediate phase carrier fusion after, be cooled to 650 ℃ and stir, churning time is 30min.After stirring finishes, be warming up to 800 ℃, the refining degasification pours in the metal type dies, makes 3% (TiB
2+ TiC)/the AM50 matrix material.
Claims (6)
1. a biphase confusion strengthens the preparation method of magnesium alloy composite, it is characterized in that technological process comprise reaction prefabricated block preparation, contain two-phase and mix dissolving diffusion and the two-phase disperse that mixes enhanced granule in magnesium alloy fused mass of the preparation of intermediate phase carrier of enhanced granule and intermediate phase carrier and distribute:
1) preparation of reaction prefabricated block:
A. prefabricated section is formed: prefabricated section is by size range Al, Ti, C and four kinds of powder constituents of B at 0.5～80 micron, and Al powder content weight percent is 28～62%, atomic ratio (B+C): Ti=2.8～3.2,
B. batch mixing: the above-mentioned powder for preparing is packed in the ball mill, and ball milling 4～30 hours mixes,
C. compression moulding: the powder that mixes is put into mould, briquetting at room temperature, pressing block density is 60～88% of this mixed powder theoretical density;
2) contain the preparation that two-phase mixes the intermediate phase carrier of enhanced granule:
Reaction prefabricated block put into vacuum or the heating unit of high-purity argon protective atmosphere is arranged, be heated to 600～800 ℃ with the heating rate of 5～30 ℃/min, cause chemosynthesis reaction, reaction product is for containing enhanced granule TiB
2, TiC and Al intermediate phase carrier;
3) dissolving diffusion and the two-phase disperse that mix enhanced granule of intermediate phase carrier in magnesium alloy substrate distributes:
A. the melting of matrix alloy: the crucible that an amount of matrix magnesium alloy will be housed is put into resistance furnace and is heated, and for preventing the oxidizing fire of magnesium alloy in the fusion process, can adopt flux to be protected or high-purity argon gas is protected, and melt temperature remains on 690～850 ℃,
B. the dissolving diffusion of intermediate phase carrier in magnesium alloy substrate: press TiB
2The weight percent that+TiC accounts for the matrix material total amount is the quality that 2～16% amount calculates corresponding intermediate phase carrier, and this intermediate phase carrier is put into 690～850 ℃ magnesium alloy fused mass, treat to stir after its dissolving diffusion,
C. melt stirring technique: whipping temp is 590～700 ℃, and churning time is 15～60min, impels two-phase to mix enhanced granule TiB through stirring
2Be distributed in the magnesium alloy fused mass with the TiC even dispersion,
D. cast obtains TiB after the refining degasification
2Strengthen magnesium alloy composite with the TiC biphase confusion.
2. biphase confusion according to claim 1 strengthens the preparation method of magnesium alloy composite; it is characterized in that in the reaction prefabricated block preparation process; its composition proportion is: Al content weight percent is 30～60%, atomic ratio (B+C): Ti=2.9～3.1, powder size are 3～74 microns.
3. biphase confusion according to claim 1 strengthens the preparation method of magnesium alloy composite, and pressing block density is 70～85% of this mixed powder theoretical density when it is characterized in that powder pressing forming.
4. biphase confusion according to claim 1 strengthens the preparation method of magnesium alloy composite; to or have when it is characterized in that preparing intermediate phase carrier that the heating rate with 10～25 ℃/min is heated to 620～780 ℃ in the heating unit of high-purity argon protective atmosphere in vacuum; cause chemosynthesis reaction, reaction product is diphase particles TiB
2, TiC and Al intermediate phase carrier.
5. biphase confusion according to claim 1 strengthens the preparation method of magnesium alloy composite, it is characterized in that preparing 3.0～15% (TiB
2+ TiC)/and the Mg matrix material, will contain corresponding two-phase and mix enhanced granule TiB
2, TiC and Al intermediate phase carrier put into 720～800 ℃ magnesium alloy fused mass dissolving diffusion.
6. biphase confusion according to claim 1 strengthens the preparation method of magnesium alloy composite, it is characterized in that whipping temp is 615～680 ℃, and churning time is 20～40min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100425720C (en) * | 2005-03-31 | 2008-10-15 | 鸿富锦精密工业（深圳）有限公司 | Creep resistant magnesium alloy materials |
| CN101161374B (en) * | 2007-11-27 | 2010-08-11 | 吉林大学 | Reactant composition for preparing multiple phase confusion TiB2-TiC ceramic particle gradient enhancement metal-based complex material |
| CN103667841A (en) * | 2014-01-16 | 2014-03-26 | 张霞 | Double-phase particle mixed enhanced magnesium alloy and preparing method of double-phase particle mixed enhanced magnesium alloy |
| CN104152766A (en) * | 2014-09-05 | 2014-11-19 | 农彩丽 | Biphase particle mixed enhanced magnesium alloy and preparation method thereof |
| CN106244867A (en) * | 2016-09-20 | 2016-12-21 | 桂林理工大学 | The preparation method of nano TiN particle enhanced aluminum-based composite material |
| CN107955889A (en) * | 2017-06-12 | 2018-04-24 | 吉林大学 | One kind utilizes interior raw nanometer TiB2The method of particle strengthening aluminium alloy |
| CN109385541A (en) * | 2018-09-14 | 2019-02-26 | 天津市大城伟业科技股份有限公司 | A method of bicycle rim is made with magnesium alloy profiles |
| CN114836670A (en) * | 2022-05-19 | 2022-08-02 | 昆明理工大学 | Method for preparing mixed ceramic phase reinforced aluminum matrix composite material through contact reaction |
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2003
- 2003-06-20 CN CN 03127091 patent/CN1228464C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100425720C (en) * | 2005-03-31 | 2008-10-15 | 鸿富锦精密工业（深圳）有限公司 | Creep resistant magnesium alloy materials |
| CN101161374B (en) * | 2007-11-27 | 2010-08-11 | 吉林大学 | Reactant composition for preparing multiple phase confusion TiB2-TiC ceramic particle gradient enhancement metal-based complex material |
| CN103667841A (en) * | 2014-01-16 | 2014-03-26 | 张霞 | Double-phase particle mixed enhanced magnesium alloy and preparing method of double-phase particle mixed enhanced magnesium alloy |
| CN103667841B (en) * | 2014-01-16 | 2015-08-05 | 张霞 | A kind of diphase particles mixed reinforced magnesium Alloy And Preparation Method |
| CN104152766A (en) * | 2014-09-05 | 2014-11-19 | 农彩丽 | Biphase particle mixed enhanced magnesium alloy and preparation method thereof |
| CN106244867A (en) * | 2016-09-20 | 2016-12-21 | 桂林理工大学 | The preparation method of nano TiN particle enhanced aluminum-based composite material |
| CN106244867B (en) * | 2016-09-20 | 2018-11-06 | 桂林理工大学 | The preparation method of nano TiN particle enhanced aluminum-based composite material |
| CN107955889A (en) * | 2017-06-12 | 2018-04-24 | 吉林大学 | One kind utilizes interior raw nanometer TiB2The method of particle strengthening aluminium alloy |
| CN107955888A (en) * | 2017-06-12 | 2018-04-24 | 吉林大学 | A kind of micro-nano TiC-TiB for aluminium alloy2Grain refiner and thinning method |
| CN107955889B (en) * | 2017-06-12 | 2019-08-27 | 吉林大学 | It is a kind of to utilize interior raw nanometer TiB2The method of particle strengthening aluminium alloy |
| CN109385541A (en) * | 2018-09-14 | 2019-02-26 | 天津市大城伟业科技股份有限公司 | A method of bicycle rim is made with magnesium alloy profiles |
| CN114836670A (en) * | 2022-05-19 | 2022-08-02 | 昆明理工大学 | Method for preparing mixed ceramic phase reinforced aluminum matrix composite material through contact reaction |
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