CN102199714A - Method for synthesizing blocky magnesium-based nano composite material by self-organized reaction - Google Patents
Method for synthesizing blocky magnesium-based nano composite material by self-organized reaction Download PDFInfo
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- CN102199714A CN102199714A CN 201110114553 CN201110114553A CN102199714A CN 102199714 A CN102199714 A CN 102199714A CN 201110114553 CN201110114553 CN 201110114553 CN 201110114553 A CN201110114553 A CN 201110114553A CN 102199714 A CN102199714 A CN 102199714A
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Abstract
The invention discloses a method for synthesizing a blocky magnesium-based nano composite material by a self-organized reaction, which comprises the following steps: (1) uniformly mixing Mg metal powder and 20 to 30 mass percent of metal oxide powder, wherein the metal oxide is the oxide of a metal having lower reducibility than magnesium; (2) forming the mixture in a mold by cold pressing, wherein the forming pressure is 400 to 600MPa; (3) sintering, wherein the temperature is constantly kept between 450 to 630 DEG C during sintering, and a flowing inert gas (such as argon and mixed gase of CO2 and SF6) is used for protection in a sintering process to prevent magnesium from being oxidized; and (4) at the end of thermal insulation, subjecting a sample to furnace cooling or quenching to obtain different intermetallic compound nano eutectic structures. In the invention, the process and equipment are simple, energy is saved, the reinforcing phase is uniformly distributed, the bonding with interface of a substrate material is firm, and cleanness and environment friendliness are guaranteed. The final hardness of the material is improved greatly, the magnetic nano particles synthesized in situ have excellent soft magnetic property, and the nano lines or nano particles formed by the reaction have high sterilizing performance.
Description
Technical field
The invention belongs to the novel preparation method of Mg-based nanocomposite.Be specifically related to a kind of method that adopts in-situ chemical reaction and self-organization phase transformation synthesizing one-dimensional magnesia nanometer line or nanometer eutectic in magnesium matrix.The Mg-based nanocomposite of physicalies such as this method is particularly useful for preparation and has the excellent mechanical mechanical property, electromagnetism and biological antibiotic function.
Background technology
Magnesium base composite material has low density, high specific tenacity and specific rigidity, good dimensional stability, low temperature superplasticity, good wear resistance, excellent damping shock absorption and capability of electromagnetic shielding, its over-all properties is better than aluminum matrix composite, and be easy to recycling, it has extremely application prospects in fields such as aerospace, automobile making, Electronic Packaging.Relevant studies show that, nano-structure strengthens magnesium base composite material and has more excellent mechanical property, the shearing resistance height, wear-resistant, electrical and thermal conductivity performance good, and the ductility of not remarkably influenced of nanometer wild phase material is so can widen its Application Areas to a great extent.
But still there are some problems in the research of magnesium base composite material now, and is not strong as the wettability between wild phase and matrix, can't form good interface in matrix material; The second phase skewness causes the regional early failure of material in wild phase shortage and enrichment; The synthesis temperature of material is higher than the fusing point of magnesium mostly, and the volatilization loss of magnesium is inevitable; The preparation technology of matrix material is too complicated, and cost is higher, can't practical application.Therefore, use significant for the novel preparation method's of magnesium base composite material research to this Development of Materials.
In-situ synthesis is a kind of novel composite material preparation method, its principle is under certain condition, by the chemical reaction between the element or between the element compound, generate the ceramic enhancement phase of one or more high strength, high elastic coefficient at the metal matrix internal in-situ, thereby reach the effect of strengthening matrix.The original position synthetic composite material is owing to have characteristics such as wild phase and basal body interface cleaning, Heat stability is good, bonding force and consistency are good, becomes one of emphasis that magnesium base composite material in recent years studies and focus.
In recent years, adopting in-situ synthesis to prepare magnesium base composite material mainly is to utilize between the simple substance powder or between simple substance powder and the magnesium matrix combination reaction takes place, original position generates wild phase, as: interpolation Ti powder and C powder prepare nano level TiC particle reinforced magnesium base compound material in magnesium alloy fused mass.But in magnesium matrix, add oxide particle and rarely have report as original wild phase and the research that generates nano-structure.With the immediate research of the present invention be: by in the magnesium melt, adding SiO
2Prepared (MgO+Mg
2Si) strengthen magnesium base composite material, visible " the reaction in synthesized Mg O/Mg of methods involving
2Si strengthens the thermodynamics and kinetics research of magnesium base composite material " (Chen Xiao, Fu Gaosheng, Qian Kuangwu, Wang Liandeng; Foundry engieering, Vol.24, No4,321～323).Yet above preparation process needs to carry out in the magnesium melt, can't avoid the volatilization of magnesium, and is comparatively difficult to the control of microstructure, and need stir to avoid the wild phase skewness melt usually, increased process complexity and cost to a great extent.
Summary of the invention
The object of the present invention is to provide the method for the synthetic block Mg-based nanocomposite of a kind of self-organization reaction, the interface cleanness of the matrix material that this method is prepared is firm, preparation technology is simple, and the hardness of material is significantly increased, generated in-situ magnetic nanoparticle has good soft magnetic performance in some system, and the magnesia nanometer line that is generated in the reaction has excellent biological antibiotic performance.
A kind of method for preparing Mg-based nanocomposite provided by the invention is characterized in that this method comprises the steps:
(1) with Mg metal-powder and massfraction be other metal oxide powder uniform mixing of 20%～30%, described other metal oxides are the oxide compound of the metal of reductibility a little less than than magnesium;
(2) powders mixture coldmoulding in mould that step (1) is obtained, forming pressure is 400MPa～600MPa;
(3) carry out sintering, holding temperature is set at 450～630 ℃ during sintering, adopts the mobile rare gas element (as argon gas, CO in the sintering process
2+ SF6 mixed gas) protection is to prevent the oxidation of magnesium;
(4) insulation finishes the back sample is carried out furnace cooling or quenching, to obtain the intermetallic compound nanometer eutectic structure of different structure.
The inventive method combines with the self-organization phase transition method in-situ chemical is synthetic, regulation and control by composition and process, the intermetallic compound eutectic structure that makes original position in the magnesium matrix generate the one dimension magnesia nanometer line or have a nanostructure style is as wild phase, this wild phase is evenly distributed in matrix, interface cleanness is firm, and preparation technology is simple.And the hardness of final material is significantly increased, and has good soft magnetic performance through reaction in synthetic nano magnetic particle, and the magnesia nanometer line that is generated in the reaction has excellent biological antibiotic performance.Particularly, technique effect of the present invention is as follows:
1) wild phase is evenly distributed, and and matrix between interface cleaning firmly
Adopted in-situ synthesis among the present invention, make in-situ chemical reaction generation one dimension magnesia nanometer line takes place between metal oxide powder and the magnesium powder, make original position self-organization generation intermetallic compound nanometer eutectic structure in the matrix by regulation and control then speed of cooling.Because this one dimension magnesia nanometer line is original position forming core, the thermodynamically stable phase of growing up in matrix, has avoided wild phase and the bad problem of matrix consistency, and in matrix uniform distribution, so interface cleanness is firm.Intermetallic compound is obtained by the nanometer eutectic reaction, compatible fabulous with matrix, interface strength of joint height, no microscopic defect existence.
2) synthesis temperature is low, technology is simple, pollution-free, the saving energy
The synthesis temperature that in-situ synthesis prepares magnesium base composite material is low, between 450～630 ℃, is lower than the fusing point of magnesium, has avoided the volatilization of magnesium.One dimension bitter earth nano wild phase generates in composite inner, does not need precursor, catalyzer and mixed gas.Intermetallic compound wild phase by nanometer eutectic self-organization phase transformation obtains has multiple nano-structure, can change the eutectic structure style by the control to alloying constituent and cooling rate.Total building-up process has equipment and technology is simple, economical, pollution-free and save advantage such as the energy.
Major equipment used in the present invention is: controlled atmosphere PID intelligent control tube furnace.
3) optimize product performance
Adopt reactive self-organizing growth method, can obtain the intermetallic compound eutectic structure that has the magnesia nanometer line of nanoscale and have the nanostructure style.Wherein, one dimension magnesia nanometer line hardness height, thermal expansivity is low, not only can be used as the matrix strengthening phase, also has excellent biological antibiotic function.And the nanometer eutectic structure is dispersed in the magnesium matrix, contains a large amount of lattice distortion, has higher surface energy, and is favourable to thermal conduction, can improve the material heat dispersion.Intermetallic compound hardness, intensity height that eutectic reaction obtains can effectively improve the mechanical mechanics property of material.Mg-based nanocomposite surface hardness value prepared among the present invention organizes the enhanced magnesium base composite material to improve 20%～50% than non-nano; In the magneticsubstance system, as Mg/Fe
3O
4, original position synthetic nanometer Fe particle has good soft magnetic performance, and coercive force is 7.493Oe, and specific saturation magnetization is 78.815emu/g, and remanent magnetism is 0.209emu/g, is very promising magnetic medicine carrier material; In addition, the one dimension bitter earth nano linear dimension that is generated in reaction is little, help kill bacteria, and surface-area is big, can adsorb chlorine in a large number, further improves sterilizing function.
Description of drawings
Fig. 1 is the transmission electron microscopy figure of Mg and CuO sample behind 450 ℃ of sintering, a) is the microstructure figure of interface zone wherein, and light areas is the MgO nano wire at the interface, and a small amount of darker regions is a Cu simple substance; B) be the selected area electron diffraction style (SAED) of interface zone, corresponding MgO crystal of diffraction ring and Cu crystal; C) the interface zone shape appearance figure for amplifying.
Fig. 2 is the scanning electron microscope microstructure figure of Mg and CuO sample behind 550 ℃ of sintering, wherein a) for the cold Mg that obtains of stove
2The Cu-Mg eutectic structure; B) be the fast cold Mg that obtains
2Cu-Mg nanometer eutectic structure.
Fig. 3 is the transmission electron microscopy shape appearance figure of Mg and NiO sample behind 550 ℃ of sintering, a) is the nanometer eutectic structure that forms around the Mg particle wherein; B) be the nanometer eutectic structure that around the MgO particle, forms.
Fig. 4 is Mg and Fe
3O
4The high resolution scanning Electronic Speculum microstructure figure of sample behind 630 ℃ of sintering a) is an one dimension magnesia nanometer line in the magnesium matrix wherein; B) be nanometer Fe particle in the magnesium matrix.
Fig. 5 is Mg and Al
2O
3The microstructure figure of sample behind 530 ℃ of sintering a) is the displaing micro tissue topography of sample behind the sintering wherein; B) be the one-dimensional nano line and the selected area electron diffraction figure thereof in MgO zone.
Embodiment
The principle of work of the inventive method is: utilize reactive self-organizing growth method, soon in-situ chemical will be synthetic combines with the self-organization phase transformation, make magnesium simple substance and metal oxide under the magnesium fusing point, in-situ chemical reaction take place, generate the one dimension magnesia nanometer line, and make the inner self-organization of matrix generate intermetallic compound nanometer eutectic structure by control to alloying constituent and cooling rate, to improve the final performance of material.
The wild phase of body material has two kinds among the present invention:
1) one dimension magnesia nanometer line wild phase.The present invention is homogeneous reaction synthesizing one-dimensional bitter earth nano line structure in magnesium matrix.Do not need precursor, catalyzer and mixed gas and synthesis temperature low when synthetic.Observing discovery one dimension magnesia nanometer line wild phase according to transmission electron microscope (TEM) is evenly distributed between the magnesium granules and chemically stable, because it is that metal oxide and matrix generation in-situ chemical reaction generate, therefore combine firmly (Fig. 1) with the interface of matrix.
2) intermetallic compound wild phase.The composition design of the molten alloy behind the in-situ chemical reaction is near eutectic.Known λ
2V=B, under condition away from equilibrium state, in order to satisfy energy condition, the lamellar spacing of nanometer eutectic, pattern, structure, two-phase volume fraction etc. are very big with the relation of cooling rate and composition, by controlling the change that can realize, realize that the self-organization of multiple intermetallic compound nanometer eutectic is constructed to nanometer eutectic structure style.The employing sem observation is found, the eutectic structure that furnace cooling obtains thick (Fig. 2), and cooling has obtained tiny nanometer eutectic structure (Fig. 3) fast.
The concrete steps of the inventive method comprise:
1) selects material system.Utilize magnesium simple substance and metal oxide (MO in the experiment
x) between replacement(metathesis)reaction, make in the matrix original position generate magnesium oxide, so the oxide compound of the metal of selective reduction a little less than than magnesium mixes as the starting materials system with the magnesium powder.Metal oxide such as CuO, NiO, Fe
3O
4Or Al
2O
3Deng.
2) according to the calphad composition proportion of the related Mg-M binary alloy system of the material system of selecting.Because intermetallic compound has high intensity, Young's modulus, toughness, good wettability and compatibility, mechanical property to the raising material is very favourable, therefore, in the composition design, in line with generating many eutectiferous principles as far as possible, with near the molten alloy composition behind the in-situ chemical reaction design zone eutectic point, and then calculate the ratio of magnesium and metal oxide according to selected one-tenth branch.As calculated, selected various composition proportion is between 20%～30%.
3) proportioning is good magnesium powder and metal oxide powder mix, and with powdered mixture coldmoulding in mould, forming pressure is 400～600MPa.In 400～600MPa scope, improve forming pressure, can improve the density of green compact, but little to the microstructure and the performance impact of sample behind the sintering.
4) use PID intelligent control tube furnace sintered specimen, holding temperature is set at 450～630 ℃ during sintering, and soaking time is 20～90min.Adopt the protection of mobile high-purity argon gas in the sintering process.
5) after the sample insulation finishes, select the different types of cooling that sample is carried out cooling process (furnace cooling or quenching).
Example:
1) preparation condition and equipment
The body material of selecting for use is that purity is 99.8% magnesium powder, and wild phase material selection purity is 99.0%～99.9% metal oxide powder.Sintering adopts controlled atmosphere PID intelligent control tube furnace, and X-ray diffractometer (XRD) is adopted in the thing identification of phases, and microstructure observation adopts environment electron microscope (SEM with analysis; LEO 1450VP) and transmission electron microscope (TEM; Philips CM 120), (Buehler 2103, IL) for hardness test employing microhardness instrument.
2) selection of sintering process
Sintering temperature is 450～630 ℃, selects different sintering temperatures according to the differing materials system, and is incubated 30～90min, makes sample furnace cooling or quenching subsequently, and concrete parameter is seen in the example.
Example 1:
Table 1 is selected material system and composition proportion:
The proportioning of table 1Mg-CuO
With powder coldmoulding under the pressure of 500MPa.
Under argon shield; green compact 1 are incubated 90min at 450 ℃; furnace cooling; through the identification of phases of XRD thing; comprise three kinds of things of Mg, MgO and Cu behind the sintering in the sample mutually; and MgO is uniformly distributed between the Mg particle at the interface, and the observation of transmission electron microscope and analytical results show that this MgO is present at the interface with the form of one-dimensional nano line, (Fig. 1).
Green compact 2 and green compact 3 are carried out furnace cooling and quenching respectively behind 550 ℃ of insulation 60min, after the XRD material phase analysis is found sintering, all comprise Mg, MgO and Mg in two samples
2Three kinds of thing phases of Cu; Find that through scanning electron microscopic observation Mg-Mg is all arranged in two samples
2Cu two-phase eutectic structure occurs, through the eutectic structure thick (Fig. 2 (a)) of furnace cooling acquisition, and tiny through cooling off the eutectic structure that obtains fast, entered nanoscale (Fig. 2 (b)).
Find that through the vickers hardness number test hardness value of green compact 2 improves 20% than pure magnesium sample, and improve 25% than green compact 2 through green compact 3 hardness values of quench treatment.The one dimension MgO nano wire that reaction generates has good germicidal action, and can adsorb chlorine in a large number, can further improve bactericidal property.
Example 2:
Table 2 is selected material system and composition proportion:
The proportioning of table 2Mg-NiO
With powder coldmoulding under the pressure of 400MPa, 500MPa respectively, to contrast.
Under argon shield, green compact are cooled off behind 550 ℃ of insulation 60min fast, after finding sintering, the XRD material phase analysis comprises Mg, MgO and Mg in the sample
2Three kinds of thing phases of Ni; Finding to generate two kinds of nanometer eutectic structures (Fig. 3) that structure is different through scanning electron microscopic observation in this sample, a) be the nanometer eutectic structure of formation around the Mg particle wherein; B) be the nanometer eutectic structure that around the MgO particle, forms.
Green compact microstructure and indistinction behind sintering of different forming pressures.
The multiple nanometer eutectic that reaction generates is not only as the wild phase of body material, and it also contains a large amount of lattice distortion, has higher surface energy, and is very favourable to thermal conduction.
Example 3:
Table 3 is selected material system and composition proportion:
Table 3Mg-Fe
3O
4Proportioning
With powder coldmoulding under the pressure of 500MPa, 600MPa respectively, to contrast.
At CO
2+ SF6 is mixed gas protected down, with green compact furnace cooling behind 630 ℃ of insulation 30min, comprises Mg, Fe, three kinds of thing phases of MgO in the sample after the XRD material phase analysis is found sintering; Through scanning electron microscopic observation with analyze to find, magnesium matrix be distributed with one dimension magnesia nanometer line and lot of F e nano particle (Fig. 4) at the interface, a) be one dimension magnesia nanometer line in the magnesium matrix wherein; B) be nanometer Fe particle in the magnesium matrix.
Green compact microstructure and indistinction behind sintering of different forming pressures.
Find that through the vickers hardness number test sample hardness value behind the sintering improves 22% than pure magnesium sample.Having good soft magnetic performance through reaction in synthetic nanometer Fe particle, is very promising magnetic medicine carrier material.One dimension MgO nano wire and Fe nano particle that reaction generates all have germicidal action.Find the one dimension MgO nano wire chlorine in the absorbed air in a large number by transmission electron microscope observing, further improve bactericidal property.
Example 4:
Table 4 is selected material system and composition proportion:
Table 4Mg-Al
2O
3Proportioning
With powder coldmoulding under the pressure of 500MPa.
At CO
2+ SF6 is mixed gas protected down, with green compact furnace cooling behind 530 ℃ of insulation 20min, comprises Mg, MgO and Mg in the sample after the XRD material phase analysis is found sintering
17Al
12Three kinds of thing phases; Through scanning electron microscope and transmission electron microscope observing and analyze and find,, a) be the displaing micro tissue topography of sample behind the sintering wherein at a large amount of one dimension magnesia nanometer lines of being distributed with at the interface of magnesium matrix (Fig. 5); B) be the one-dimensional nano line in MgO zone.
Find that through the vickers hardness number test sample hardness value behind the sintering has improved nearly 50% than pure magnesium hardness value.And the one dimension MgO nano wire that is generated in the reaction can improve the bactericidal property of material to a great extent.
The present invention not only is confined to above-mentioned embodiment; persons skilled in the art are according to embodiment and the disclosed content of accompanying drawing; can adopt other multiple embodiment to implement the present invention; therefore; every employing mentality of designing of the present invention; do some simple designs that change or change, all fall into the scope of protection of the invention.
Claims (2)
1. a method for preparing Mg-based nanocomposite is characterized in that, this method comprises the steps:
(1) with Mg metal-powder and massfraction be other metal oxide powder uniform mixing of 20%～30%, described other metal oxides are the oxide compound of the metal of reductibility a little less than than magnesium;
(2) mixture coldmoulding in mould that step (1) is obtained, forming pressure is 400MPa～600MPa;
(3) carry out sintering, holding temperature is set at 450～630 ℃ during sintering, adopts the mobile protection of inert gas in the sintering process, to prevent the oxidation of magnesium;
(4) insulation finishes the back sample is carried out furnace cooling or quenching, to obtain the intermetallic compound nanometer eutectic structure of different structure.
2. the method for preparing Mg-based nanocomposite according to claim 1 is characterized in that: in the step (3), the soaking time in the sintering process is 20～90min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104524869A (en) * | 2014-12-15 | 2015-04-22 | 西安建筑科技大学 | MgO/Fe-Cr-Ni porous composite filter material and preparation method thereof |
| CN105779839A (en) * | 2016-05-09 | 2016-07-20 | 天津理工大学 | Self-protection degradable MgO/Mg-Zn-Ca biological composite material |
| CN107385253A (en) * | 2017-06-28 | 2017-11-24 | 山东正凯机械科技有限公司 | A kind of preparation method of the wear-resisting magnesium alloy brake disc of nanocrystalline enhancing |
| CN107760946A (en) * | 2017-10-26 | 2018-03-06 | 中南大学 | A kind of Biological magnesium alloy containing nano magnesia and Nano Silver and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837392A (en) * | 2006-04-03 | 2006-09-27 | 重庆大学 | Composite material of magnesium alloy and method for preparing the same |
| CN101386926A (en) * | 2007-09-14 | 2009-03-18 | 清华大学 | Method for preparing Mg-based compound material and preparation apparatus |
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2011
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837392A (en) * | 2006-04-03 | 2006-09-27 | 重庆大学 | Composite material of magnesium alloy and method for preparing the same |
| CN101386926A (en) * | 2007-09-14 | 2009-03-18 | 清华大学 | Method for preparing Mg-based compound material and preparation apparatus |
Non-Patent Citations (1)
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| 《中国优秀硕士学位论文全文数据库 基础科学辑》 20090515 谭娟 镁基复合材料的反应性自组织合成与表征 A005-55 1-2 , 第05期 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104524869A (en) * | 2014-12-15 | 2015-04-22 | 西安建筑科技大学 | MgO/Fe-Cr-Ni porous composite filter material and preparation method thereof |
| CN105779839A (en) * | 2016-05-09 | 2016-07-20 | 天津理工大学 | Self-protection degradable MgO/Mg-Zn-Ca biological composite material |
| CN107385253A (en) * | 2017-06-28 | 2017-11-24 | 山东正凯机械科技有限公司 | A kind of preparation method of the wear-resisting magnesium alloy brake disc of nanocrystalline enhancing |
| CN107760946A (en) * | 2017-10-26 | 2018-03-06 | 中南大学 | A kind of Biological magnesium alloy containing nano magnesia and Nano Silver and preparation method thereof |
| CN107760946B (en) * | 2017-10-26 | 2019-08-02 | 中南大学 | A kind of Biological magnesium alloy and preparation method thereof containing nano magnesia and nano silver |
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Application publication date: 20110928 |