WO2004062837A1 - マグネシウム複合粉末およびその製造方法ならびにマグネシウム基複合材料およびその製造方法 - Google Patents
マグネシウム複合粉末およびその製造方法ならびにマグネシウム基複合材料およびその製造方法 Download PDFInfo
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- WO2004062837A1 WO2004062837A1 PCT/JP2003/017083 JP0317083W WO2004062837A1 WO 2004062837 A1 WO2004062837 A1 WO 2004062837A1 JP 0317083 W JP0317083 W JP 0317083W WO 2004062837 A1 WO2004062837 A1 WO 2004062837A1
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- magnesium
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- magnesium alloy
- fine powder
- composite material
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/148—Agglomerating
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- the present invention relates to a magnesium-based composite material and a method for producing the same.
- the present invention relates to a magnesium composite powder as a starting material for producing a particle-dispersed magnesium-based composite material by solid-phase reaction synthesis and a method for producing the same, and a magnesium-based composite material using the composite powder and a method for producing the same About. Background art
- Magnesium alloy is known as the lightest material and its utility value is high. On the other hand, magnesium alloys are pointed out as having low hardness, low rigidity, low wear resistance, and low corrosion resistance.
- S i) A method for producing a magnesium-based composite material in which particles are dispersed is disclosed. Specifically, when a magnesium alloy containing a high concentration of silicon (S i) is injection-molded in a semi-molten state, magnesium silicide (M g 2 ) is formed by a reaction between magnesium (M g) in the matrix and silicon. S i).
- Japanese Patent Application Laid-Open No. 8-41564 discloses a magnesium-based composite material in which magnesium silicide (Mg 2 Si) particles and silicon carbide (SiC) particles are dispersed by a forging method. Have been. Also, Japanese Patent Application Laid-Open No. 2000-173532 discloses a magnesium-based composite material in which spherical magnesium silicide (Mg 2 Si) particles are dispersed by a manufacturing method. . In the prior art described in each of the above publications, magnesium silicide (Mg 2 S i) particles dispersed in a magnesium-based composite material have a particle diameter of 100 / m 2 due to grain growth in the process of solidifying from a dissolved or semi-dissolved state.
- magnesium (Mg) and silicon (Si) react with each other to form a magnesium alloy.
- Fine magnesium silicide (Mg 2 S i) particles are uniformly dispersed in the substrate.
- a magnesium-based composite material in which fine magnesium silicide (Mg 2 S i) particles are uniformly dispersed by using a solid-phase reaction synthesis method between magnesium (Mg) and silicon (S i) is used.
- the silicon particles in the mixed solid before reaction do not remarkably grow and become coarse during the solid-phase reaction process, the size of the silicon (S i) particles before reaction is almost equal to that of magnesium silicide (Mg 2 S i) with the size of the particles. Therefore, the ability to finely disperse silicon particles in the mixed solidified solids leads to the miniaturization of magnesium silicide (Mg 2 S i) particles in the magnesium-based composite material, which in turn leads to a higher strength composite material. It leads to higher functionality.
- Hard particles such as magnesium silicide (Mg 2 Si) are finely and uniformly The properties of the magnesium-based composite material are improved by dispersing it in the magnesium alloy matrix.
- Mg 2 Si magnesium silicide
- magnesium (Mg) alloy material When the size of the magnesium alloy powder or the magnesium alloy chip becomes significantly larger than that of silicon (Si) particles, a two-layer separation phenomenon occurs in the mixture of the magnesium alloy starting material and the silicon particles, and only fine silicon particles are removed. Segregation in one place causes problems. In order to avoid this problem, it is conceivable to use a fine magnesium alloy material as a starting material. However, since magnesium has an active property that is easily oxidized among metals, a fine magnesium alloy powder of about several tens of ⁇ m may cause explosion in the atmosphere. Considering the danger point, it is extremely difficult in practice to use fine magnesium alloy powder as a starting material.
- the present invention has been made to solve the above problems, and an object of the present invention is to disperse compound particles generated by a solid-phase reaction with magnesium, which is a main component, uniformly in a magnesium alloy matrix. It is to provide a magnesium based composite material. Another object of the present invention is to provide a magnesium composite powder as a starting material for producing the magnesium-based composite material as described above.
- Still another object of the present invention is to provide a method capable of economically producing the above-mentioned magnesium-based composite material.
- Still another object of the present invention is to provide a method capable of efficiently producing a magnesium composite powder as a starting material for a magnesium-based composite material as described above.
- the size thereof is preferably about 500 5 ⁇ to 5 ⁇ from the viewpoint of avoiding explosion in the atmosphere.
- the size of the fine powder composed of a component that reacts with magnesium to produce a compound is about 0.5 ⁇ to 50 ⁇ um.
- fine powder is adhered to the surface of the magnesium alloy coarse particles as the main component.
- the particle size of the fine powder is about 1Z10 to 1/10000 of the magnesium alloy coarse particles, which is much finer than that of the magnesium alloy coarse particles.
- the magnesium composite powder according to the present invention is a starting material for producing a particle-dispersed magnesium-based composite material by solid-phase reaction synthesis.
- Magnesium composite powder is composed of magnesium alloy coarse particles, which are the main components constituting the base of the magnesium alloy, and a component that reacts with magnesium to generate a compound, and fine powder adhered to the surface of the magnesium alloy coarse particles. Is provided.
- Fine powder adhering to Maguneshiumu alloy coarse grain surface is preferably silicon (S i), silica (S I_ ⁇ 2), selected from the group consisting of ⁇ -alumina (A 1 2 0 3) and aluminum (A 1) Containing at least one or more powder particles.
- the magnesium alloy coarse particles have a particle size of 100 ⁇ m to 5 mm, and the fine powder has a particle size of 100 ⁇ m or less. More preferably, the particle size of the magnesium alloy coarse particles is from 500 ⁇ m to 2 mm, and the particle size of the fine powder is 0.5 ⁇ ! ⁇ 50 / xm.
- the bedding powder is attached to the surface of the magnesium alloy coarse particles via a binder.
- the fine powder and the magnesium alloy coarse particles are mechanically combined.
- the fine powder is attached to the surface of the magnesium alloy coarse particles via oil.
- the magnesium-based composite material according to the present invention is produced using the above-described magnesium composite powder, and a reaction product of the magnesium alloy coarse particles and the fine particles is dispersed in the magnesium alloy base.
- the reaction product preferably, M g 2 S i, M g O, were selected A 1 3 M g 2, M g 1 7 A 1 1 2 Oyobi ⁇ ! 1 2 0 group or al of four Contains at least one or more compounds.
- the magnesium based composite material preferably comprises graphite powder as a solid lubricant.
- the content of the graphite powder is desirably 0.5% to 3% by weight based on the magnesium-based composite material.
- the total content of the reaction products in the magnesium alloy base is 20% or less on a weight basis. More preferably, the total content of reaction products is from 5% to: L 0% by weight.
- the method for producing a magnesium composite powder according to the present invention includes the following steps.
- the method for producing a magnesium alloy according to the present invention includes the following steps.
- the warm plastic working is an extrusion method with an extrusion ratio of 20 or more. More preferably, the extrusion ratio of the extrusion method is 35 or more.
- Compound particles are preferably, M g 2 S i, M g 0, A 1 3 M g 2, M g 1 7 A 1! 2 and M g A 1 2 0 4 at least one selected from the group consisting of It includes the above compounds.
- the fine powder adheres to the surface of the magnesium alloy coarse particles using a binder.
- the step of adhering the fine powder includes mixing the fine powder into the pinda solution, and spraying and drying the binder solution containing the fine powder on the magnesium alloy coarse particles.
- the fine powder is attached to the surface of the magnesium alloy grit via oil.
- the vaporization temperature of the oil in an inert gas atmosphere or a non-oxidizing atmosphere is 400 ° C. or less.
- the adhesion of the oil is performed, for example, as follows. First, a magnesium alloy coarse powder is filled in a container. Subsequently, oil is put into the container, and the container is rotated, vibrated, and oscillated to uniformly adhere the oil to the surface of the magnesium alloy coarse powder. Subsequently, the fine powder is put into the container, and the container is again rotated, vibrated, and oscillated, so that the fine powder adheres to the surface of the magnesium alloy coarse powder via oil.
- the amount of the oil added is preferably 0.2 to 1%, more preferably 0.3 to 0.6% by weight based on the magnesium alloy coarse powder.
- Oil adhesion may be performed as follows. First, a magnesium alloy coarse powder is filled in a container. Subsequently, the oil and balls are put into the container, and the container is rotated, vibrated, and oscillated to uniformly adhere the oil to the surface of the magnesium alloy coarse powder. Subsequently, the fine powder is charged into the container, and the container is again rotated, vibrated, and positively moved so that the fine powder is attached to the surface of the magnesium alloy coarse powder via oil. In yet another embodiment, the fine powder is mechanically bonded to the surface of the magnesium alloy grit. BRIEF DESCRIPTION OF THE FIGURES
- FIG. 1 is an illustrative view showing one example of a method of attaching a fine powder to a surface of a magnesium alloy coarse particle using a binder.
- FIG. 2 is an illustrative view showing another example of a method for attaching fine powder to a surface of a magnesium alloy coarse particle using a binder.
- FIG. 3 is an illustrative view showing still another example of the method of attaching fine powder to the surface of the magnesium alloy coarse particles using a binder.
- FIG. 4 is an illustrative view showing one example of a magnesium composite powder in which fine powder is adhered to the surface of a magnesium alloy coarse particle.
- FIG. 5 is an illustrative view showing one example of a method of mechanically bonding fine powder to a surface of a magnesium alloy coarse particle.
- FIG. 6 is an illustrative view showing another example of a method of mechanically bonding fine powder to the surface of a magnesium alloy coarse particle.
- FIG. 7 is an illustrative view showing still another example of the method of mechanically bonding fine powder to the surface of magnesium alloy coarse particles.
- FIG. 8 is an illustrative view showing another example of a magnesium composite powder in which fine powder is adhered to the surface of a magnesium alloy coarse particle.
- FIG. 9 is a diagram showing an example of a method for producing a magnesium-based composite material.
- FIG. 10 is a diagram showing another example of a method for producing a magnesium-based composite material.
- FIG. 11 is a diagram schematically showing the structure of the compacted solid before the solid phase reaction.
- FIG. 12 is a diagram schematically showing the structure of the magnesium alloy after the solid-phase reaction.
- FIG. 13 is a micrograph showing a structure of a magnesium composite powder in which silica powder is mechanically bonded and adhered to the surface of AZ91.
- FIG. 14 is a diagram showing a method for simply evaluating the adhesion state of silicon powder.
- FIG. 15 is a diagram showing the evaluation results of the silicon powder adhesion state.
- the magnesium composite powder is a starting material for producing a particle-dispersed magnesium-based composite material, and includes a magnesium alloy coarse particle and a fine powder attached to the surface of the magnesium alloy coarse particle.
- Chip-shaped magnesium alloy coarse particles can be obtained by cutting magnesium alloy billets (ingots).
- Lumpy magnesium alloy coarse particles are obtained by collecting a large lump from an ingot by a pulverizer or the like, and mixing and pulverizing the lump with a ball mill or the like.
- the particle size of the magnesium alloy coarse particles is 100 ⁇ n! About 5 mm is preferable. More preferably, 500 n! ⁇ 2 mm. If the particle size of the magnesium alloy coarse particles is less than 100 ⁇ m, the possibility of dust explosion during the handling process increases. On the other hand, when the particle size of the magnesium alloy coarse particles exceeds 5 mm, when the obtained magnesium composite powder is compacted and solidified, cracks and cracks occur on the surface and corners of the solidified body, and a good solidified body is formed. There is a possibility that it cannot be obtained. Of the magnesium alloy coarse particles obtained by the above-mentioned production method, those which passed through a 5 mm mesh by the sieving method but did not pass through a ⁇ ⁇ m mesh were used as raw materials.
- the magnesium alloy coarse particles include powders, chips, and lumps.
- particle size refers to the maximum length in each form. The particle size is measured by direct observation with a stereoscopic microscope, an optical microscope, a scanning electron microscope, or the like, by a magnifying projector, or by using a particle size distribution measuring instrument used for measuring the particle size of powder.
- Magnesium alloy coarse particles form the basis of the magnesium matrix composite material
- the alloy components include existing magnesium alloys such as AZ31 (Mg-3% A1-1% Zn / weight basis) and AZ91 (Mg-9% A1-1-1% Zn / Etc. can be applied. There are no particular restrictions on the alloy components.
- the fine powder adhering to the surface of the magnesium alloy coarse particles generates compound particles by solid-phase reaction synthesis with magnesium.
- Such fine-grained powder silicon (S i), silica (S i 0 2), ⁇ -alumina (A 1 2 0 3) and at least one or more kinds of powder selected from the group consisting of aluminum Niumu (A 1) Is used.
- silicon powder Mg 2 Si is obtained.
- silica powder Mg 2 S i and Mg O are obtained.
- a 1 3 Mg 2 and Z or Mg 17 A 1 12 and / or Mg A 1 2 0 4 is obtained in addition to the Mg O.
- Al 3 Mg 2 and / or Mg 17 A 1 12 are obtained.
- Alumina has two types of crystal structures, ⁇ and ⁇ , but the present inventor has found that ⁇ -alumina can produce the above compound particles by reaction with magnesium. Since ⁇ -alumina is more stable than ⁇ -alumina, it was confirmed that it did not react with the magnesium alloy in the solidus temperature range of about 600 ° C or lower. Therefore, it is necessary that the alumina fine powder adhering to the surface of the magnesium alloy coarse particles has a ⁇ crystal structure.
- each fine powder is 0.5 ⁇ ! 1100 ⁇ m. Since the fine powder reacts with magnesium in the solid phase temperature range, the particle size of the compound particles generated almost matches the particle size of the fine powder before the reaction. In order to improve the properties such as strength, hardness, and abrasion resistance of the magnesium-based composite material, the smaller the particle size of the compound particles dispersed in the base material is, the better the dispersion is. Therefore, it is desirable that the particle size of the fine powder selected from silicon (Si), silica (Si 2 ), y-alumina (A 1 2 3 ), and aluminum (A 1) used as the raw material is small. If the particle size of the fine powder exceeds 100 m, the properties of the magnesium-based composite material deteriorate.
- the particle size of the fine powder falls below 0.5 ⁇ , Due to the effect of electrostatic attraction or water adsorbed on the surface, the fine powders are firmly agglomerated to form a coarse powder having a particle size exceeding 100 / m. As a result, a problem arises when the compound particles dispersed in the base material of the magnesium-based composite material become coarse particles exceeding 100 ⁇ m, which induces a deterioration in characteristics.
- the dispersed compound particles in order to maintain high toughness while maintaining high toughness, which is one of the excellent features of magnesium alloys, it is desirable that the dispersed compound particles have a particle size of 50 ⁇ m or less.
- the particle size of the fine powder is preferably 0.5 ⁇ to 10 ⁇ .
- a method of measuring the particle size distribution from the degree of light transmission by transmitting light while the powder is stirred and dispersed in glycol or an aqueous solution can be used.
- Fine powder is uniformly dispersed and adhered to the surface of the magnesium alloy coarse particles to obtain a magnesium composite powder.
- this composite powder as a starting material and subjecting the composite powder to compaction, heating, and warm plastic working, a magnesium-based composite material in which fine compound particles are uniformly dispersed in the substrate can be obtained. .
- Methods for uniformly dispersing and adhering the fine powder on the surface of the magnesium alloy coarse particles include: a method of adhering the two via a binder, a method of adhering the two via oil, and a method of applying both by applying external force. There is a method of mechanically coupling.
- the binder is preferably a binder having a water-soluble property or a solubility in an organic solvent and selected from water-soluble dextran, saccharides, celluloses, and synthetic polymers.
- a binder having a water-soluble property or a solubility in an organic solvent selected from water-soluble dextran, saccharides, celluloses, and synthetic polymers.
- the water-soluble binder polyvinyl alcohol (PVA), polybierpyrrolidone (PVP), polyvinyl methyl ether (PVM), polyacrylamide, methylcellulose (MC), starch and the like can be used.
- Organic solvent-soluble binders include polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), hydroxypropylcellulose (HPC), hydroxypropylmethylcellulose, ethylcellulose (EC), and acetylcellulose. Can be used.
- PVP polyvinylpyrrolidone
- PEG polyethylene glycol
- HPC hydroxypropylcellulose
- EC hydroxypropylmethylcellulose
- EC ethylcellulose
- acetylcellulose acetylcellulose
- Figures 1 to 3 show adhesion by a binder using a wet granulator or spray dryer. 4 shows an example of a method.
- a mixture 2 of a magnesium alloy coarse particle and a fine powder is charged into a container 1, and hot air 3 is supplied from a lower portion of the container 1 to float the mixture 2.
- the binder solution 4 is sprayed onto the mixture 2 from above and the binder is applied to the surface of each particle, and simultaneously dried at high temperature.
- the fine powder 8 adheres and bonds to the surface of the magnesium alloy coarse particles 7 via the binder 9.
- the binder solution 4 is sprayed from the bottom perpendicular to the direction of the air flow while the mixture 2 of the magnesium alloy coarse particles and the fine particles is suspended in the container 1 at a relatively low air volume. I have.
- the binder solution 6 sprayed on the magnesium alloy coarse particles 5 contains fine powder. While sufficiently stirring the binder solution 6 in order to suppress the precipitation of fine powder in the binder solution 6, the binder solution 6 is sprayed from the upper portion of the container 1 into the magnesium alloy coarse particles 5 by spraying. Note that the binder solution 6 may be sprayed from below as shown in FIG. By this method, the fine powder can be uniformly attached to the surface of the magnesium alloy coarse particles.
- the fine powder is remarkably smaller than the magnesium alloy coarse particles, and when the mixture of both is suspended by strong wind, the fine powder tends to rise above the coarse particles in the granulator (container). .
- the reason is considered to be that the specific surface area of the fine powder is larger than that of the coarse powder. Therefore, there is a possibility that the fine powder and the coarse magnesium powder may be separated from each other in the space inside the granulator, and in such a case, it takes a long time to uniformly adhere the fine powder to the surface of the magnesium alloy coarse particles. I need it. In order to avoid such a problem, it is effective to mix the fine powder in the binder solution in advance.
- an oil such as oleic oil may be used instead of the binder.
- a predetermined magnesium composite powder is obtained by attaching an oil such as oleic acid oil to the magnesium alloy coarse particles, adding a fine powder, and mixing with a pole mill or the like.
- the gas has a vaporization temperature of 400 ° C. or less.
- the oil is attached, for example, as follows. First, a magnesium alloy coarse powder is filled in a container. Subsequently, oil is poured into the container, and the container is rotated, vibrated, and oscillated to uniformly adhere the oil to the surface of the magnesium alloy coarse powder. Subsequently, the fine powder is charged into the container, and the container is again rotated, vibrated, and positively moved so that the fine powder is attached to the surface of the magnesium alloy coarse powder via oil.
- the amount of the oil added is preferably 0.2 to 1%, more preferably 0.3 to 0.6% by weight based on the magnesium alloy coarse powder. If the amount of oil added is less than 0.2%, most of the fine powder is separated without adhering to the surface of the magnesium alloy coarse particles. On the other hand, even if the oil content exceeds 1%, the adhesion effect is not improved, and the oil remains in the magnesium-based composite material even after heat treatment in a later step, and the strength and elongation at break are reduced. Such a problem arises.
- a more preferable addition amount of the oil is 0.3 to 0.6% by weight. If the added amount is 0.3% or more, no separation of the fine powder occurs at all, and the fine powder can completely adhere to the surface of the coarse powder. When the addition amount is 0.6% or less, oil does not remain inside the magnesium-based composite material, and the time required for heat treatment for decomposing and removing the oil can be shortened. It is preferable in terms of economy.
- the structure of the magnesium composite powder obtained as described above is substantially the same as that shown in FIG. Instead of binder 9, oil will remain.
- FIGS 5 to 7 show the method of mechanically bonding the fine powder to the surface of the magnesium alloy coarse particles.
- a mixture 2 of a magnesium alloy coarse particle and a fine powder is charged into a machine called a roller compactor 10.
- a granulated material 14 is obtained in which fine powder is mechanically bonded and adhered to the surface of the magnesium alloy coarse particles.
- the granulated material 14 is passed through a pulverizing / sieving machine 13 to obtain a magnesium composite powder 15 having a predetermined size and shape.
- fine powder 8 is mechanically bonded and adhered to the surface of magnesium alloy coarse particles 7.
- a pair of cylindrical rollers 16 and 17 are used instead of a pair of gears.
- a mixture 2 of magnesium alloy coarse particles and fine particles is conveyed to a pair of cylindrical rollers 16 and 17 on a belt conveyor 18. and that c should be noted, may be subjected to feeding the mixture at a subscription user feeder from the side instead of using the belt conveyor.
- the machine used to mechanically bond and adhere the fine powder to the surface of the magnesium alloy coarse particles is not limited to the roller compactor.
- a magnesium composite powder in which fine powder is mechanically bonded to a coarse particle surface can be obtained by a ball mill or a rolling mill.
- graphite powder which is a solid lubricant, is mixed with the above-mentioned magnesium composite powder and added to the magnesium-based composite material.
- the type of graphite powder either natural black mouth or artificial graphite can be applied.
- shape There is no particular limitation on the shape, and any shape of black powder, such as spheres and scales, can be used.
- the amount of the graphite powder to be added is preferably in the range of 0.5 to 3% by weight based on the total amount of the magnesium-based composite material. If it is less than 0.5%, the effect of reducing the coefficient of friction cannot be obtained, while if it exceeds 3%, there arises a problem that the strength of the magnesium-based composite material is significantly reduced. .
- the magnesium-based composite material is obtained by compacting and solidifying the above-described magnesium composite powder, and then heating and holding the solidified body in a predetermined temperature range.
- the solid phase including the redox reaction between the magnesium component of the magnesium alloy coarse particles constituting the magnesium composite powder and the fine powder adhered and bonded to the coarse particle surface Reaction synthesis proceeds, and the resulting compound particles become Disperse evenly in it.
- Mg 2 S i, MgO, A 1 3 Mg 2, Mg 17 A 1 12 and Mg A 1 2 0 at least selected from the group consisting of 4 one or more Of the compound.
- Mg 2 S i, A 1 3 Mg 2, Mg 17 A 1 12 mainly has the effect of improving the strength of the magnesium alloy, the hardness, the wear resistance.
- Mg 2 Si has higher rigidity than other compound particles, it has a role of improving the rigidity of the composite material by dispersing it in the base material of the magnesium-based composite material.
- MgO oxides such as Mg A 1 2 0 4 is hardness than other compound particles is low, because, there is the effect to relax the counterpart material, dispersed in friction sliding the material mixture of the composite material to its It plays the role of reducing the coefficient of friction when moving.
- the total content of these compound particles in the magnesium-based composite material is desirably 20% or less on a weight basis. If the total content exceeds 20%, the toughness of the magnesium based composite material is significantly reduced. A more preferable range of the total content is 5% to 10%. If such a range is satisfied, a magnesium-based composite material having more excellent strength and toughness can be obtained.
- FIG. 9 and FIG. 10 show steps of a method for producing a magnesium-based composite material.
- the difference between the two manufacturing methods lies in the process of manufacturing the magnesium-based composite powder.
- the magnesium alloy coarse particles and the fine powder are weighed and blended, and then the two are adhered and bonded.
- the fine powder is mixed in the binder solution in advance, and the mixed solution containing the fine powder is sprayed onto the magnesium alloy coarse particles, and then the two are adhered and bonded. It is.
- methods for adhering and bonding the fine powder to the surface of the magnesium alloy coarse particles include a method via a binder, a method via oil, and a method for mechanically bonding by applying an external force.
- a magnesium composite powder in which fine powder is dispersed and adhered and bonded to the surface of the magnesium alloy coarse particles is obtained.
- the relative density of the green compact is preferably 80% or more. If the relative density is less than 80%, the strength of the solidified compact decreases, and there is a possibility that damage, chipping, cracking, etc. may occur during the transportation process.
- FIG. 11 schematically shows the structure of the compacted solid before the solid-phase reaction. As shown in the figure, the fine powder 41 is uniformly dispersed in the magnesium alloy base 40.
- FIG. 12 schematically shows the structure of the magnesium alloy after the solid-phase reaction synthesis. As shown in the figure, a reaction product 42 and a reaction product 43 are dispersed in a magnesium alloy base material 40.
- the heating atmosphere of the green compact is preferably an inert gas atmosphere and preferably a non-oxidizing gas atmosphere.
- the heating temperature depends on the type of fine powder to be mixed. Regardless of the type of fine powder used, the solid-state reaction with the magnesium alloy coarse particles involves an exothermic behavior, so that the reaction start temperature and the reaction end temperature can be accurately determined using a differential calorimeter. Therefore, fine compound particles can be generated by setting the reaction end temperature determined by such a differential calorimeter as the heating / holding temperature of the solidified compact. It should be noted that the method of the present invention is characterized by suppressing the coarsening and grain growth of compound particles generated by utilizing a solid-phase reaction at a temperature lower than the melting point of magnesium. Less than ° C.
- the used oil When the compacted solid is heated in an inert gas atmosphere or a non-oxidizing atmosphere using a magnesium composite powder produced via oil, the used oil is decomposed and vaporized to compact the compact. Remove from body. At that time, if the vaporization temperature of the oil exceeds 400 ° C., there is a problem that the oil remains inside the compact and the strength and the elongation at break are reduced. Therefore, it is desirable that the oil used for attaching the fine powder has a vaporization temperature of 400 ° C. or less in an inert gas atmosphere or a non-oxidizing atmosphere.
- the relative density be 98% or more.
- the relative density of the green compact is about 80% to 90%, so in the present invention, after the above-mentioned heating step, warm plastic working is performed to densify. Extrusion, forging, rolling and the like can be applied as the warm plastic working method.
- the warm extrusion method is a method suitable for producing a rod-shaped or pipe-shaped magnesium alloy material.
- the extrusion ratio it is desirable to set the extrusion ratio to 20 or more. In particular, when the extrusion ratio is set to 35 or more, the compound particles produced by the solid-phase reaction synthesis are more finely pulverized, and the same effect can be obtained when the particles are uniformly dispersed in the magnesium-based composite material.
- a magnesium-based composite material exhibiting mechanical properties such as high strength, high hardness, and high rigidity, and excellent frictional sliding properties can be obtained. Particularly, it is possible to obtain a magnesium-based composite material which can exhibit a small friction coefficient.
- Such a magnesium-based composite material has the above-mentioned properties and also has the effect of reducing the weight. Therefore, parts and machine parts for automobiles, motorcycles and bicycles, structural parts, industrial robot arms, medical equipment, nursing care aids Applicable to baby carriage products.
- AZ31 magnesium alloy coarse powder having a maximum particle size of 1.5 mm, a minimum particle size of 550 m, and an average particle size of 870 ⁇ m was used as a starting material for forming a base for producing a magnesium alloy.
- silicon (S i), shea silica (S I_ ⁇ 2) was prepared fine powder of y alumina (A 1 2 0 3) and aluminum (A 1).
- Table 1 shows the particle size (maximum / average / minimum) of these powders measured by the laser diffraction / scattering method. ⁇ table 1 ⁇
- Each mixed powder is put into a wet granulation device, and the mixed powder is suspended and stirred by warm air (held at 75 ° C) from the bottom of the device and rotating blades at the bottom.
- a PVA aqueous solution was sprayed from a spray gun installed at the bottom.
- a magnesium composite granulated powder in which each fine powder was adhered to the surface of the AZ31 coarse powder by the PVA binder serving as a paste was obtained.
- Table 2 shows the appearance results of the state of adhesion of the fine powder to the surface of the AZ31 coarse powder when the spray application amount of the PVA aqueous solution to the whole mixed powder was changed.
- Example 2 AZ91 with a maximum particle diameter of 4.6 mm, a minimum particle diameter of 680 ⁇ m, and an average particle diameter of 3.8 mm produced by cutting was used as a starting material that constitutes the base material for producing a magnesium alloy. A magnesium alloy coarse chip was prepared. On the other hand, fine particles of silicon (Si) shown in Example 1 were prepared as additive particles.
- the AZ91 coarse-grained chips were weighed to 95% and the Si fine-grained powders were weighed to 5% on a weight basis.
- An aqueous solution of PVP (polyvinylpyrrolidone) having a concentration shown in Table 3 was prepared as a binder solution, and the weighed Si fine powder was mixed with the aqueous solution.
- the aqueous solution of PVP was 20% by weight based on the whole mixed powder.
- the AZ91 alloy chips are put into the wet granulation apparatus, and the AZ91 alloy chips are stirred by the hot air (held at 75 ° C) from the bottom of the apparatus and the rotating blades at the bottom, and The PVP aqueous solution containing the fine Si powder was sprayed from a spray gun installed at the bottom. At this time, in order to suppress precipitation of the Si powder in the aqueous solution of PVP, the aqueous solution of PVP was sufficiently stirred by a screw during fogging.
- the PVP binder acts as a glue to obtain a magnesium composite powder with the Si fine powder adhered to the surface of the AZ91 alloy chip.
- Table 3 shows the appearance of the adhesion of the Si fine powder to the AZ91 alloy chip surface under each spray condition.
- Example 2 The AZ91 magnesium alloy coarse chip used in Example 2 and the fine powder of silica (Sio 2 ) shown in Example 1 were prepared. Each was weighed and mixed so that 70% of AZ91 coarse-grain chips and 30% of silica fine-grain powder were based on weight. The mixture was subjected to mechanical granulation using a vertical roller compactor. Here, a roller having a gear shape was used. The roller speed at the outer periphery was kept constant at 1 Omsec, and the load between gears was set at about 1 OKg OK.
- Fig. 13 shows the results of observing the appearance of the obtained granules with a scanning electron microscope.
- the granulated product obtained by the roller compactor was a magnesium composite powder in which silica fine powder was mechanically adhered uniformly to the AZ91 chip surface.
- Example 2 Were prepared and fine powder of ⁇ -alumina as shown in A Zeta 91 alloy tip as Example 1 used in Example 2 (A 1 2 0 3) . Each was weighed so that 96% of AZ91 alloy chips and 4% of alumina fine powder were based on weight.
- AZ91 chips with oleic acid oil were added to a ball mill together with steel balls (SUJ2) with a diameter of 1 Omm and mixed for about 5 minutes. In this process, the oleic acid oil was uniformly attached to the chip surface.
- Table 4 shows the appearance results of the adhesion state of the fine alumina powder to the AZ91 alloy chip surface under each condition.
- Example 1 Guneshiumu coarse powder and silicon used in Example 1 (S i), silica (S i 0 2), was prepared fine powder of ⁇ -alumina (A 1 2 0 3) and aluminum (A 1). Each powder was blended so as to have the chemical composition (weight basis) shown in Table 5, and a magnesium composite powder was produced by the vertical roller compactor used in Example 3.
- a cylindrical compact having a diameter of 36 mm was prepared by cold compaction using each magnesium composite powder. Each solid was heated and maintained at a temperature of 550 ° C. for 5 minutes in a tubular furnace into which nitrogen gas was introduced, and then immediately subjected to warm extrusion at an extrusion ratio of 36 to obtain an extruded rod having a diameter of 6 mm.
- the differential calorimetric analysis shows that the magnesium alloy heated and extruded at 380 ° C for 5 minutes, which is 100 to 150 ° C lower than the exothermic reaction temperature, and then hot-extruded is subjected to XRD bonding. The results are shown in Samples 8 and 9.
- Fine powders of 1 2 3 ) and ⁇ -alumina (1 2 0 3 ) were prepared. A shown in Table 6
- Each powder was blended so as to have a chemical composition (weight basis), and a magnesium composite powder was produced using the vertical roller compactor used in Example 3.
- a cylindrical compact having a diameter of 36 mm was prepared by cold compaction using each magnesium composite powder.
- Each solidified body was heated and maintained at the temperature shown in Table 6 for 5 minutes in a tubular furnace into which nitrogen gas was introduced, and immediately thereafter, was subjected to warm extrusion at an extrusion ratio of 36 to obtain an extruded rod having a diameter of 6 mm.
- X-ray diffraction (XRD) was performed on the obtained extruded material, and the generated compound phase was identified. Table 6 shows the results.
- the A31 alloy coarse powder used in Example 1 was prepared as a magnesium alloy base powder, while silicon (Si) fine powder having a particle diameter shown in Table 7 was prepared as an additive particle.
- a magnesium composite powder composed of AZ31 alloy coarse particles and Si fine powder was prepared such that the Si content was 4 ° / 0 of the whole on a weight basis.
- oleic acid oil was previously applied to the AZ31 coarse particles by the method described in Example 4, and then the Si powder was coated on the surface of the AZ31 coarse particles with a ball mill. Was attached.
- a columnar compact of 36 mm in diameter was prepared from each mixed powder, and each compact was heated and maintained at 550 for 5 minutes in a tubular furnace into which nitrogen gas had flowed, and then immediately heated at an extrusion ratio of 36.
- An extruded rod having a diameter of 6 mm was obtained by performing an extrusion process. X-ray diffraction was performed on each of the magnesium alloys after extrusion, and as a result, the formation of Mg 2 S i particles by the solid-phase reaction was confirmed in each case.
- the particle size of the Si powder to be added satisfies the appropriate range described above.
- the magnesium alloy obtained by extrusion as the particle size becomes smaller. Has improved tensile strength.
- the Si particle diameter is 50 ⁇ m or less, an increase in elongation in addition to the strength is observed.
- Si fine powder of 10 ⁇ m or less the elongation at break of the magnesium alloy is remarkable. Improved.
- Sample No. 7 contains fine Si powder with a particle size of less than 0.5 ⁇ m, so that agglomeration of the fine particles forms a structure in which coarse Mg 2 Si is dispersed in the magnesium alloy base material. As a result, the tensile strength and elongation at break of the magnesium alloy are reduced. did.
- Example 1 AZ31 coarse powder and silica (Si 2 ) fine powder used in Example 1 were prepared. In addition, graphite powder having an average particle size of 3 ⁇ was used as a starting material as a solid lubricating component. Table 8 shows the mixing ratio of each powder.
- silica powder and graphite powder As a method for attaching silica powder and graphite powder to the surface of AZ31 coarse particles, as in the wet granulation method shown in Example 2, the silica powder and graphite powder are added to a 2% PVA aqueous solution in advance, and granulation is performed. An aqueous PVA solution was applied to the surface of coarse AZ31 particles by a spray gun from the lower part of the apparatus to produce a magnesium composite powder.
- a column-shaped compact of 4 Omm in diameter was prepared from each mixed powder, and each compact was heated and maintained at 550 ° C for 5 minutes in a tubular furnace into which nitrogen gas was introduced. Extrusion was performed to obtain an extruded rod having a diameter of 8 mm. X-ray diffraction of each extruded magnesium alloy confirmed that Mg 2 S i particles were generated by solid-state reaction in each case.
- a pin-shaped wear test specimen (diameter 7.8 mm) was collected from the extruded material to measure the friction coefficient by a friction test.
- S35C steel was used as the disc material on the other side, the pressing load was 500N, the sliding speed was lraZs, and the test time was 30 minutes continuously.
- Engine lubricating oil (10W30) was dripped from the upper part of the pin-shaped test piece under wet lubrication conditions in which lubricating oil was always present at the sliding interface between the pin-shaped test piece and the disk test piece. The test was performed. Table 8 shows the results of calculating the friction coefficient from the measured friction torque.
- the AZ31 alloy coarse powder used in Example 1 was prepared as a magnesium alloy base powder.
- fine particles of silicon (Si) (maximum particle diameter: 24 ⁇ m, average particle diameter: 8 ⁇ m, minimum particle diameter: 1 ⁇ m) were prepared as additive particles, and the composition was determined on a weight basis.
- Si silicon
- a magnesium composite powder composed of AZ31 alloy coarse particles and Si fine powder was prepared so as to obtain AZ31-4% Si.
- oleic acid oil was previously applied to the AZ31 coarse particles by the method described in Example 4, and then the Si powder was applied to the surface of the AZ31 coarse particles by a ball mill. Was attached.
- the amount of the oleic acid oil added was 0.3% by weight based on the AZ31 alloy powder.
- the Si powder was uniformly attached to the surface of the AZ31 coarse particles, and the separated Si powder was in a good adhesion state without being observed.
- a columnar compact (diameter: 91%) having a diameter of 36 mm was prepared from the mixed powder, and each compact was heated and maintained at 550 ° C for 5 minutes in a tubular furnace into which nitrogen gas was introduced. Immediately, warm extrusion was performed to obtain an extruded rod.
- the extrusion ratio R (diameter of solidified product / diameter of extruded material) was the square of the extrusion ratio, and the extrusion ratio used here is shown in Table 9. X-ray diffraction was performed on each of the extruded magnesium alloys, and as a result, formation of Mg 2 S i particles by solid-state reaction was confirmed in each case. Tensile test specimens were collected from each extruded material by machining and subjected to a tensile test at room temperature. Table 9 shows the results. [Table 9]
- both the tensile strength and the elongation at break of the extruded material increase as the value of the extrusion ratio increases, and particularly when the extrusion ratio exceeds 35, these mechanical properties increase remarkably.
- the extrusion ratio is less than 20, as in sample No. 5, the tensile strength and elongation at break of the extruded material decrease.
- the AZ31 alloy coarse powder and the silicon powder used in Example 9 were prepared, and both powders were weighed such that the composition of both was AZ31-4% Si on a weight basis.
- AZ31 coarse powder is filled in a cylindrical vinyl container, and 0.1, 0.25, and 0.4% by weight of oleic acid oil are added to this. Rotation and vibration were applied for 15 minutes. After that, the container was filled with Si powder, and the mixture was again subjected to mixing treatment by rotation and vibration for 15 minutes to produce three types of predetermined magnesium composite powder.
- FIG. 14 shows a method for easily evaluating the adhesion state of silicon powder. Evaluation of the adhesion state is performed as follows.
- Figure 15 shows the evaluation results of the silicon powder adhesion status.
- the Si powder hardly remained on the white paper.
- S i powder is AZ 3 (1) It is recognized that it is firmly attached to the surface of the alloy coarse particles.
- 0.1% by weight of oleic acid oil of Comparative Example (c) was used, most of the Si powder remained on the surface of the white paper and adhered to the surface of the AZ31 coarse powder. And it is recognized that they are separated.
- the present invention can be used for parts for automobiles, two-wheeled vehicles, bicycles, machine parts, structural parts, industrial robot arms, medical equipment, nursing care aids, baby carriage supplies, and the like.
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Abstract
Description
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Priority Applications (4)
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US10/541,758 US20060057015A1 (en) | 2003-01-08 | 2003-12-26 | Magnesium composite powder, method for producing same, magnesium base composite material and method for producing same |
AU2003292731A AU2003292731A1 (en) | 2003-01-08 | 2003-12-26 | Magnesium composite powder, method for producing same, magnesium base composite material and method for producing same |
EP03768386A EP1586395A4 (en) | 2003-01-08 | 2003-12-26 | MAGNESIUM COMPOUND POWDER, METHOD OF MANUFACTURING THEREOF, MAGNESIUM BASED COMPOSITE MATERIAL AND METHOD OF PRODUCTION THEREOF |
JP2004566307A JPWO2004062837A1 (ja) | 2003-01-08 | 2003-12-26 | マグネシウム複合粉末およびその製造方法ならびにマグネシウム基複合材料およびその製造方法 |
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JP2003-002602 | 2003-01-08 |
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US (2) | US20060057015A1 (ja) |
EP (1) | EP1586395A4 (ja) |
JP (1) | JPWO2004062837A1 (ja) |
CN (1) | CN100431742C (ja) |
AU (1) | AU2003292731A1 (ja) |
WO (1) | WO2004062837A1 (ja) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110153407A (zh) * | 2019-06-10 | 2019-08-23 | 张国忠 | 一种Al2O3陶瓷颗粒增强镁合金基复合材料及制备方法 |
US11866808B2 (en) | 2020-03-23 | 2024-01-09 | Seiko Epson Corporation | Method for manufacturing thixomolding material |
US11865609B2 (en) | 2020-03-23 | 2024-01-09 | Seiko Epson Corporation | Method for manufacturing powder-modified magnesium alloy chip |
Families Citing this family (7)
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CN103451464B (zh) * | 2013-08-27 | 2015-11-25 | 朱育盼 | 一种Mg2Si增强的Mg合金复合材料 |
CN104117685B (zh) * | 2014-07-30 | 2016-08-24 | 金堆城钼业股份有限公司 | 一种钼酸钠掺杂钼粉的制备方法 |
JP6981094B2 (ja) * | 2017-08-15 | 2021-12-15 | 三菱マテリアル株式会社 | マグネシウム系熱電変換材料、マグネシウム系熱電変換素子、及び、マグネシウム系熱電変換材料の製造方法 |
JP2022153979A (ja) * | 2021-03-30 | 2022-10-13 | セイコーエプソン株式会社 | チクソ成形用材料、チクソ成形用材料の製造方法およびチクソ成形体 |
JP2022153982A (ja) * | 2021-03-30 | 2022-10-13 | セイコーエプソン株式会社 | チクソ成形用材料、チクソ成形用材料の製造方法およびチクソ成形体 |
CN113430437A (zh) * | 2021-06-03 | 2021-09-24 | 辽宁银捷装备科技股份有限公司 | 一种高强度铸造镁合金及其制备方法 |
CN114959336B (zh) * | 2022-01-30 | 2023-09-15 | 安徽工业大学 | 一种触变注射成形用镁基复合材料的制备方法及其制得的镁基复合材料 |
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2003
- 2003-12-26 CN CNB2003801085045A patent/CN100431742C/zh not_active Expired - Fee Related
- 2003-12-26 US US10/541,758 patent/US20060057015A1/en not_active Abandoned
- 2003-12-26 JP JP2004566307A patent/JPWO2004062837A1/ja active Pending
- 2003-12-26 EP EP03768386A patent/EP1586395A4/en not_active Withdrawn
- 2003-12-26 AU AU2003292731A patent/AU2003292731A1/en not_active Abandoned
- 2003-12-26 WO PCT/JP2003/017083 patent/WO2004062837A1/ja active Application Filing
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110153407A (zh) * | 2019-06-10 | 2019-08-23 | 张国忠 | 一种Al2O3陶瓷颗粒增强镁合金基复合材料及制备方法 |
US11866808B2 (en) | 2020-03-23 | 2024-01-09 | Seiko Epson Corporation | Method for manufacturing thixomolding material |
US11865609B2 (en) | 2020-03-23 | 2024-01-09 | Seiko Epson Corporation | Method for manufacturing powder-modified magnesium alloy chip |
Also Published As
Publication number | Publication date |
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JPWO2004062837A1 (ja) | 2006-05-18 |
US20080213118A1 (en) | 2008-09-04 |
EP1586395A4 (en) | 2008-03-19 |
EP1586395A1 (en) | 2005-10-19 |
CN100431742C (zh) | 2008-11-12 |
CN1735472A (zh) | 2006-02-15 |
US20060057015A1 (en) | 2006-03-16 |
AU2003292731A1 (en) | 2004-08-10 |
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